Category: 101-84-8

In 2020.0 RUSS J PHYS CHEM A+ published article about BINARY-MIXTURES; DENSITY in [Yakovlev, I. G.; Garkushin, I. K.; Kolyado, A., V] Samara State Tech Univ, Samara 443001, Russia in 2020.0, Cited 19.0. The Name is Diphenyl oxide. Through research, I have a further understanding and discovery of 101-84-8. HPLC of Formula: C12H10O

A theoretical and experimental study is performed for liquid-solid phase equilibria in the two-component diphenyl oxide-n-hexadecane system. The results show that this system is eutectic. Two means are chosen for the theoretical study of the system: the Schroder-Le Chatelier equations and the original UNIFAC system. Experimental studies are made via differential thermal analysis on a DSC unit. Results from the theoretical and experimental studies are presented in the formT-xdiagrams of the system. The theoretical and experimental data are compared to one another. Each way of calculating is assessed, and recommendations are made for their application. The eutectic coordinates (melting point and composition) are determined experimentally. The following values are determined experimentally for a eutectic melt: the enthalpy of melting; density at 25 degrees C; kinematic viscosity in the temperature range of 25 to 50 degrees C; flash point in an open cup; boiling point, and refractive index in the temperature range of 25 to 40 degrees C. The composition of the eutectic melt can be used in industry as a heat transfer fluid.

HPLC of Formula: C12H10O. About Diphenyl oxide, If you have any questions, you can contact Yakovlev, IG; Garkushin, IK; Kolyado, AV or concate me.

Reference:
Ether – Wikipedia,
,Ether | (C2H5)2O – PubChem

I found the field of Chemistry very interesting. Saw the article Regioselective C-H Amidation of (Alkyl)arenes by Iron(II) Catalysis published in 2019. HPLC of Formula: C12H10O, Reprint Addresses Tian, JS; Loh, TP (corresponding author), Nanjing Tech Univ NanjingTech, Jiangsu Natl Synerget Innovat Ctr Adv Mat SICAM, SCME, IAS, 30 South Puzhu Rd, Nanjing 211816, Jiangsu, Peoples R China.; Loh, TP (corresponding author), Nanyang Technol Univ, Sch Phys & Math Sci, Div Chem & Biol Chem, Singapore 637371, Singapore.; Loh, TP (corresponding author), Univ Sci & Technol China, Dept Chem, Hefei 230026, Anhui, Peoples R China.. The CAS is 101-84-8. Through research, I have a further understanding and discovery of Diphenyl oxide

A nondirected amidation reaction of aromatic C-H bond was developed under iron(II) catalysis, using sulfonyl azides as the nitrogen source. The reaction displayed a broad substrate scope and good regioselectivities in the aspects of aromatic ring vs alkyl chain and different aromatic position of (alkyl)arenes. This method provided a new protocol for the synthesis of some aromatic amines, which were hard to achieve in a previous report.

About Diphenyl oxide, If you have any questions, you can contact Ding, Y; Zhang, SY; Chen, YC; Fan, SX; Tian, JS; Loh, TP or concate me.. HPLC of Formula: C12H10O

Reference:
Ether – Wikipedia,
,Ether | (C2H5)2O – PubChem

An article Recent history of persistent organic pollutants (PAHs, PCBs, PBDEs) in sediments from a large tropical lake WOS:000461270900030 published article about POLYCYCLIC AROMATIC-HYDROCARBONS; HEAVY-METALS; RIVER-BASIN; CHAPALA; MEXICO; EXPOSURE; VERACRUZ; POPS; GULF; CONTAMINATION in [Feliciano Ontiveros-Cuadras, Jorge; Sanchez-Cabeza, Joan-Albert] Univ Nacl Autonoma Mexico, Inst Ciencias Mar & Limnol, Unidad Acad Proc Ocean & Costeros, Ciudad Univ, Mexico City 04510, DF, Mexico; [Carolina Ruiz-Fernandez, Ana; Hascibe Perez-Bernal, Libia; Paez-Osuna, Federico] Univ Nacl Autonoma Mexico, Inst Ciencias Mar & Limnol, Unidad Acad Mazatlan, Mazatlan 82040, Mexico; [Sericano, Jose] Texas A&M Univ, Geochem & Environm Res Grp, 833 Graham Rd, College Stn, TX 77845 USA; [Dunbar, Robert B.; Mucciarone, David A.] Stanford Univ, Earth Syst Sci, Stanford, CA 94305 USA in 2019.0, Cited 74.0. Recommanded Product: Diphenyl oxide. The Name is Diphenyl oxide. Through research, I have a further understanding and discovery of 101-84-8

Pb-210-dated sediment cores and surface sediments from Lake Chapala (LC), Mexico, were analyzed to assess the temporal trends in concentrations and fluxes of persistent organic pollutants (POPs: PAHs, PCBs and PBDEs). Total sediment concentrations of PAHs (95-1,482 ng g(-1)), PCBs (9-27 ng g(-1)) and PBDEs (0.2-2.5 ng g(-1)) were indicative of moderate to intense contamination. The POP concentrations have progressively increased since the 1990s. The light molecular weight PAHs, and the prevalence of PCB congeners with low-chlorination levels (e.g., di- to tri-CB) and low-to medium-brominated (tri- to penta-BDE) PBDEs in most sections of the sediment profiles, suggested that these POPs have most likely reached these sediments by long-range atmospheric transport from distant sources; although the significant presence of heavier PAH, PCB and PBDE congeners in the topmost sediments, indicate that other nearby and local sources (soil erosion from the catchment, urban and industrial wastewaters discharges, as well as navigation) might have also contributed to the recent input of POPs to LC. Taking into account the relevance of LC as regional freshwater supply and commercial fishing ground, the potential risk posed by the organic contaminated sediments to the biota and human population should not be underestimated.

About Diphenyl oxide, If you have any questions, you can contact Ontiveros-Cuadras, JF; Ruiz-Fernandez, AC; Sanchez-Cabeza, JA; Sericano, J; Perez-Bernal, LH; Paez-Osuna, F; Dunbar, RB; Mucciarone, DA or concate me.. Recommanded Product: Diphenyl oxide

Reference:
Ether – Wikipedia,
,Ether | (C2H5)2O – PubChem

Adding a certain compound to certain chemical reactions, such as: 101-84-8, name is Diphenyl oxide, belongs to ethers-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 101-84-8, Formula: C12H10O

EXAMPLE 1; A reactor is configured from a 1-liter Morton flask with a mechanical stirrer, thermometer, a 60 mL addition funnel, and a distillation column. The condenser from the distillation column is connected to a H2O trap. A small N2 purge is added to the line from the condenser to the H2O trap. The reactor is charged with AlCl3 and bromine. The addition funnel is charged with diphenyl oxide. The reactor is heated to 55 C. and the diphenyl oxide is added drop-wise supersurface to the bromine. The reactor is heated by a mantle. After all of the diphenyl oxide has been added, the addition funnel is replaced with a Br2 feed line. After several minutes of refluxing, the distillation of Br2 (containing HBr) is initiated. At the same time, the Br2 feed is initiated. As needed, the feed rate of the Br2 is adjusted so that the volume in the reactor remains fairly constant. After the distillation and concurrent replacement feed of Br2 are conducted for an hour, the liquid mixture is cooled to 55 C., some deionized H2O is added, and most of the Br2 is distilled off. When most of the Br2 is gone, more deionized water is added. The remaining Br2 is then distilled. The remaining mixture is cooled to 60 C., and a portion of an aqueous 25% NaOH solution is added to make the pH 13-14. The resultant mixture is filtered and washed well with deionized water. A sample is subjected to GC analysis and then is oven dried.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Diphenyl oxide, and friends who are interested can also refer to it.

Reference:
Patent; ALBEMARLE CORPORATION; US2008/58558; (2008); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 101-84-8, name is Diphenyl oxide, A new synthetic method of this compound is introduced below., name: Diphenyl oxide

EXAMPLE 1; Catalyzed Bromination [0047] A reactor was configured from a 1 -liter Morton flask with a mechanical stirrer, thermometer, 60 mL addition funnel, and fractionation column (10″ x 1″ (ca. 25.4 cm x 2.54 cm) with 5 mm x 5 mm Raschig rings) topped by a O0C reflux condenser. The outlet of the condenser was connected to a H2O trap. A small N2 purge was added to the line from the condenser to the H2O trap. The reactor was charged with 3.5 g OfAlCl3 and 1577g of bromine (containing 11 ppm H2O). The addition funnel was charged with 47.04 g of diphenyl oxide.The reactor was heated to 550C and the diphenyl oxide was added drop-wise supersurface. The time for the initiation of the diphenyl oxide addition was noted. The reactor was heated by a mantle. Twenty-seven minutes into the diphenyl oxide feed, half of the diphenyl oxide had been added and the reaction mass temperature was 560C. One and a quarter hours after the diphenyl oxide feed was initiated, all of the diphenyl oxide had been added and the reaction mass temperature was 570C. The compressor on the refrigeration system was shut off to allow slow warm-up of the condenser. The reaction mass was refluxed through the fractionation column. At one hour and 18 minutes after feed initiation, the reaction mass temperature was 590C. Two hours and three minutes after diphenyl oxide feed initiation the condenser water was at 2O0C and the reaction temperature was at 610C. At two hours and seven minutes after feed initiation, the condenser water was at 3O0C. Thirty two minutes later the addition funnel was replaced with a N2 inlet. A slow N2 purge of the reactor was started. The reaction mass temperature was 610C. The N2 purge was at 100 mL/min into the vapor space of the reactor. Four hours and fifty minutes after the initiation of the diphenyl oxide feed, the reaction mass temperature was 610C and the condenser water was at 370C. At six hours and 15 minutes after the initiation of the diphenyl oxide feed the reaction mass was cooled to 550C, 350 mL deionized H2O was added, the fractionation column was removed, and the reactor was set for distillation. Br2 was distilled off. When most of the Br2 was gone 150 mL more deionized water was added. The remaining Br2 was distilled off to 1000C. The remaining mixture was cooled to 6O0C, and 30 mL of 25% NaOH was added to pH 13-14. The resultant mix was filtered and washed well with deionized water. A sample was subjected to GC analysis. The GC trace showed the product to contain 0.21% of the first nonabromodiphenyl oxide peak (deemed to be meta- and para-hydrogen isomers), 0.24% of the second nonabromodiphenyl oxide peak (deemed to be the ortho-hydrogen isomer) and 99.54% of decabromodiphenyl oxide. The sample was oven dried.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; ALBEMARLE CORPORATION; WO2008/27776; (2008); A2;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Reference of 101-84-8,Some common heterocyclic compound, 101-84-8, name is Diphenyl oxide, molecular formula is C12H10O, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

The reactor was charged with 3.16 g of AlCl3 and 711 g of bromine. Diphenyl oxide (46.1 g, 0.271 mol) and the Br2/Cl2 mixture (BrCl) were cofed to the reactor during 124 minutes at 55 C to 57 C. The rate of addition was at a proportion of about 8.2 g Br2/Cl2 mixture (BrCl) per gram of DPO, such that the addition of both was completed at the same time. The mixture in the reactor was refluxed for 10 minutes after the cofeeds had ended, and deionized H2O was added. The reactor was set for distillation. The halogen (mostly Br2, but also comprised of BrCl and Cl2) was distilled off. When most of the halogen was gone, more deionized water was added. The remaining halogen was distilled off to 1000C. The remaining mixture was cooled to 6O0C, and 30 mL of 25% NaOH was added to pH 13-14. The resultant mixture was filtered and washed well with deionized water. A sample was subjected to GC analysis. The GC trace showed the product to contain 0.26% Br9DPO (meta and para hydrogen isomers only), 2.52% Br9ClDPO, and 97.2% Br10DPO. None (less than 0.02%) of the ortho hydrogen isomer of Br9DPO was detected. The sample was oven dried. [0043] The drawings show illustrative GC traces formed using the recommended gas chromatographic procedure described hereinabove. In these traces, the abscissa is time in minutes and the ordinate is the detector response. A copy of the GC trace of the product formed in Example 1 appears as Fig. 1. In Fig. 1, the peak at 1.358 represents the area percentage of what is deemed to be the meta and para isomers of nonabromodiphenyl oxide. No peak for the ortho-isomer of nonabromodiphenyl oxide was observed. The peaks at 2.103 and 2.200 were deemed to be Br9ClDPO isomers. The peak at 2.649 represents the area percentage of decabromodiphenyl oxide.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Diphenyl oxide, its application will become more common.

Reference:
Patent; ALBEMARLE CORPORATION; WO2008/27780; (2008); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Reference of 101-84-8, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 101-84-8, name is Diphenyl oxide belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

EXAMPLE 6; Preparation of Partially brominated DPO[0056] To the 500 mL flask (equipped as described in Example 4) containing 47.3 g of DPO was added over about 10 minutes, 28.0 g of bromine with stirring and cooling at room temperature. Catalyzed Bromination [0057] In a 1 -liter jacketed flask equipped with mechanical stirrer, Friedrich condenser(water cooled at about 250C), and with a 1/32-inch diptube but without a fractionation column were placed 3.8 g of AlCl3 and 885 g of bromine. After a feed time of about 7.25 hours, all of the partially brominated DPO had been fed from the flask. The reaction temperature was maintained at 56.30C to 57.20C throughout the addition. The reaction mixture was refluxed for 4 minutes as the temperature rose to 58.40C, then 450 mL of water was added and the reactor was set for distillation. The product was distilled to 1700F (about 770C) and 312 g of bromine was collected. The water layer was decanted from the reactor, 400 mL of water was added, stirred, and discarded. Then 400 mL of water and 10 g of NaOH were added, the mixture was stirred well and product was collected and water washed on a filter. GC analysis showed the product was composed of 99.71% of decabromodiphenyl oxide, and 0.034 and0.259% of the first and second nonabromodiphenyl oxide isomers, respectively. The product was placed in a 1250C oven and after drying overnight weighed 252.0 g. EXAMPLE 7Preparation of Partially brominated DPO [0058] To the 500 mL flask (equipped as described in Example 4) containing 49.1 g of DPO was added over aboutlO minutes, 29.7 g of bromine. This was purged with nitrogen to remove HBr. Catalyzed Bromination[0059] In a 1 -liter jacketed flask equipped as in Example 6 (no fractionation column) were placed 3.8 g of AlCl3 and 884 g of bromine. The mixture was heated to 59C and a feed of the partially brominated DPO formed above was initiated. The feed through the 1/32-inch diptube was set at a rate of about 0.21 mL per minute. All the partially brominated DPO was added over 3 hours and 23 minutes, The reaction mixture had been maintained at a temperature of 56.10C to 57.10C throughout the addition time reflux was continued for about 10 more minutes as the temperature rose to 59.60C. Then 450 mL of water was added to the reaction mixture and the reactor was set for distillation. The mixture was distilled to 770C and 294.5 g of bromine was collected. The mixture was worked up as in Example 6. GC analysis of the product showed 99.59% of decabromodiphenyl oxide and 0.11% and 0.296% of first and second nonabromodiphenyl oxide peaks, respectively. Present in the product were a few “lumps”. One was removed and a GC showed it contained 99.61% of decabromodiphenyl oxide and 0.100 and 0.291% of the first and second nonabromodiphenyl oxide isomers, respectively. The product was oven dried. EXAMPLE 8Preparation of Partially brominated DPO [0060] To the 500 mL flask (equipped as in Example 4) containing 49.00 g of DPO was added 31.4 g of bromine over about 10 minutes. Then the mixture was purged with nitrogen. Catalyzed Bromination[0061] In a 1 -liter jacketed flask, equipped as in Example 6, were placed 3.82 g OfAlCl3 and 988 g of bromine The mixture was heated to 56.O0C and addition of the partially brominated DPO begun at a feed rate of about 0.18 mL per minute. This feed was maintained for a period of about 4 hours with the temperature fluctuating between 53.O0C and 54.O0C. The mixture was allowed to reflux for about another 7 minutes with the temperature reaching about 600C. Then, 450 mL of water was added to the reaction mixture and the reaction vessel was set for distilling bromine. The distillation was conducted to 770C whereby an amount of 400.2 g of bromine was recovered. Product was isolated as in Example 5 and oven dried. GC analysis showed 0.093% and 0.471% of the first and second nonabromodiphenyl oxide peaks, respectively, and 99.436% of decabromodiphenyl oxide. After drying over the weekend the product weighed 260.1 g.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, Diphenyl oxide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ALBEMARLE CORPORATION; WO2008/27776; (2008); A2;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Electric Literature of 101-84-8, These common heterocyclic compound, 101-84-8, name is Diphenyl oxide, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

EXAMPLE 3; Preparation of Partially brominated DPO[0050] To the 500 mL 4-neck flask equipped as in Example 2 was added 732g of Br2. Molten diphenyl oxide (49.3 g) was added dropwise at bromine reflux over 40 minutes. The solution was refluxed (O0C condenser) 45 minutes longer. Catalyzed Bromination[0051] To the 1-liter flask, equipped as in Example 2, were added 4.0 g of AlCl3 and 595 g of bromine. This mixture was brought to reflux through the fractionation column and the contents of the 500 mL flask were pumped in at -0.5 niL/min via the 1/16″ (ca. 0.16 cm) O. D., 1/32″ (ca. 0.08 cm) LD. diptube subsurface to the resulting reaction mass. The reaction mass temperature was 590C. The reaction mass was kept at hard reflux throughout the solution addition. The temperature of the cooling water on condenser was 170C. Eight hours later, all of the contents of the 500 mL flask had been pumped into the 1 -liter flask. About 5 mL of bromine was added to the 500 mL flask and this bromine was pumped into the 1 -liter flask. The reaction mass was then refluxed 15 minutes longer with a N2 purge (about 100-200 niL/min. down the diptube). The reaction mass was cooled partially, and 50O mL of H2O was added and the reactor was set for distillation. Bromine was distilled to 1000C and the reaction mass was cooled to 6O0C. Excess 5% NaOH added to pH 12. The solid product was collected and washed well with H2O. A sample was analyzed by GC. GC analysis showed the product to contain 0.017% of the first nonabromodiphenyl oxide peak (meta and para isomers), 0.031% of the second nonabromodiphenyl oxide peak (ortho isomer) and 99.95% of decabromodiphenyl oxide. The remainder of the product was dried overnight at 13O0C and, after drying, weighed 263 g. EXAMPLE 4; Preparation of Partially brominated DPO [0052] To 50.0 g of DPO in a 500 rnL flask equipped with magnetic stirrer, addition funnel, thermometer, and condenser was added 29 g of bromine dropwise over 30 minutes. The reactor was cooled in a water bath. When all the bromine had been added, the reactor was purged with nitrogen to facilitate pumping and prevent HBr breakout in the line. Catalyzed Bromination [0053] In a 1-liter 4-neck Morton flask were placed 4.05 g of AlCl3 and 1230 g of bromine.The flask was equipped with 1/32-inch (ca. 0.08 cm) LD. diptube (subsurface) and a fractionation column as described in Example 2 and topped with a tap water cooled Friedrich condenser. This mixture was brought to reflux and the DPO mixture was pumped into the reactor via the 1/32-inch diptube. Reaction temperature was 590C. Heating was such that bromine vapor rose to about 1A of the height of the condenser before totally condensing. The temperature of the cooling water exiting the condenser was 25.6C. After 6 hours and 58 minutes of feeding, all of the DPO had been added except for about Ig remaining in the flask. The diptube was removed and the reaction mixture was refluxed 10 minutes longer. Water (500 mL) was added and the reactor was set for bromine distillation. Bromine was distilled to a reaction temperature of 1000C. 658 g of bromine was collected. The reactor was cooled,5% NaOH was added to pH of about 13, and the product was collected and washed. GC analysis showed the product to contain 0.020% of the first nonabromodiphenyl oxide peak (meta and para isomers), 0.080% of the second nonabromodiphenyl oxide peak (ortho isomer) and 99.90% of decabromodiphenyl oxide. The product was dried overnight at 1300C. After drying overnight the product weighed 265.2 g. EXAMPLE 5Preparation of Partially brominated DPO[0054] To the 500 mL flask (equipped as described in Example 4) containing 51.67 g ofDPO was added 30.0 g of bromine over about 10 minutes with cooling in a water bath. After stirring for 15 minutes this mixture was nitrogen sparged to remove HBr.Catalyzed Bromination[0055] In a 1 -liter jacketed 4-neck flask equipped with a thermocouple, 1/32-inch LD. dip tube, mechanical stirrer and 9 inch x 1 inch (ca. 22.8 cm x 2.54 cm) column (packed with 5 mm x 5 mm Raschig rings) and topped with a water-cooled Friedrich condenser, and heated by circulating hot water through the jacket, the water temperature being controlled to give the desire reaction temperature, were placed 4.0 g OfAlCl3 and 1240 g of bromine. This mixture was heated to 56.70C and DPO addition initiated. After a DPO feed time of 9 hours and 42 minutes, during which time the reaction temperature was maintained mainly at 56.10C to 57.10C, the feed was stopped and the mixture was refluxed 5 minutes longer under a nitrogen purge of the reaction flask. Then 500 mL of water was added and the flask was set for distillation. 617 Grams of bromine was distilled to a temperature of 800C. The stirrer in the flask was stopped and the resultant water phase was decanted. The solids were washed with 500 mL of water and the water was decanted. Then 500 mL of water and 10 g of NaOH were added to the solids and the mixture …

The synthetic route of 101-84-8 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 101-84-8,Some common heterocyclic compound, 101-84-8, name is Diphenyl oxide, molecular formula is C12H10O, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Example 12 (comparative)Decabromodiphenyl ether – Bromination of Deca completely dissolved in bromine.; The solubility of Deca in bromine was determined as 2.64 g Deca in 100 g bromine at 200C.To a 1 liter round bottomed flask equipped with a mechanical stirrer, a dropping funnel, a thermocouple and a reflux condenser was added 22 g of non milled Deca (content 97.1 %) and 1642 g bromine to produce a 1.32 % solution. AlBr3, 14.1 g, was added and the mixture was heated at reflux for 5 hours. After cooling to room temperature, water, 250 ml, was carefully added. The bromine was distilled and an additional 520 g of water was added. The solid was filtered and dried and consisted of 99.6 % Deca.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Diphenyl oxide, its application will become more common.

Electric Literature of 101-84-8, These common heterocyclic compound, 101-84-8, name is Diphenyl oxide, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Comparative Example; A 500 milliliter four-neck round bottom flask was fitted with a mechanical stirrer, a double walled reflux condenser, a thermocouple, a temperature controller, a heating mantle, and a syringe pump fitted with a Teflon needle. The flask was vented to a water trap for collection of by-product hydrogen bromide. Dry bromine (929.5 grams, 5.82 moles, 200% excess) was charged into the reaction flask, followed by 4.1 grams of aluminum chloride (0.031 mole). The reaction was stirred for 5 minutes.Addition of 33.0 grams (0.19 mole) of diphenyl ether was initiated to the bromine-catalyst mixture at a temperature of 25C. The diphenyl ether addition was maintained at a constant rate by use of a syringe pump over a period of about 180 minutes. The reaction temperature was allowed to increase by way of exotherm to about 35C. Additional heat was applied after the diphenyl ether addition had been completed, and the reaction temperature increased to about 59C within about 20 minutes. After 180 minutes of post addition heating, the heat input was removed and the reaction allowed to cool to room temperature in about 90 minutes.A two liter four-neck round bottom flask was fitted with a mechanical stirrer, a distilling head, a double walled reflux condenser, a thermocouple, a temperature controller, and a heating mantle. One liter of water and the reaction slurry were charged to the flask and the excess bromine was distilled off until a temperature of 100C was achieved.Decabromodiphenyl ether was filtered from the aqueous slurry, washed with water, and dried at 100 C. in a forced air oven.Gas chromatographic analysis of the resulting product showed decabromodiphenyl ether 96.93 area percent, nonabromodiphenyl ether isomers totaling 2.79%, octabromodiphenyl ether isomers totaling 0.25%, and heptabromodiphenyl ether isomers totaling 0.02%.; Example 1; A two liter four-neck round bottom flask was fitted with a mechanical stirrer, a double walled reflux condenser, a thermocouple, a temperature controller, a heating mantle, and a syringe pump fitted with a Teflon needle. The flask was vented to a water trap for collection of by-product hydrogen bromide. Dry bromine (3,410 grams, 21.34 moles, 1000% excess) was charged into the reaction flask, followed by 17.9 grams of aluminum chloride (0.13 mole). The reaction was stirred for five minutes.Addition of 33.0 grams (0.19 mole) of diphenyl ether was initiated to the bromine-catalyst mixture at a temperature of 25 C. The diphenyl ether addition was maintained at a constant rate by use of a syringe pump over a period of about 60 minutes. The reaction temperature was allowed to increase by way of exotherm to about 35 C. Additional heat was applied after the diphenyl ether addition had been completed, and the reaction temperature increased to about 59 C. within about 20 minutes. After about 60 minutes of post addition heating, the heat input was removed and the reaction allowed to cool to room temperature in about 90 minutes.A three liter four-neck round bottom flask was fitted with a mechanical stirrer, a distilling head, a double walled reflux condenser, a thermocouple, a temperature controller, and a heating mantle. One liter of water and the reaction slurry were charged to the flask and the excess bromine was distilled off until a temperature of 100 C. was achieved.Decabromodiphenyl ether was filtered from the aqueous slurry, washed with water, and dried at 100 C. in a forced air oven.Gas chromatographic analysis of the resulting product showed decabromodiphenylether 99.95 area percent, nonabromodiphenyl ether isomers totaling 0.05%, with no other isomers present.; Example 2; The procedure of Example 1 was repeated except that the amount of aluminum chloride was reduced to 6.2 grams (0.047 mole).Gas chromatographic analysis of the resulting product showed decabromodiphenylether 99.90 area percent and nonabromodiphenyl ether 0.1%, with no other isomers present.; Example 3; A two liter four-neck round bottom flask was fitted with a mechanical stirrer, a double-walled reflux condenser, a thermocouple, a temperature controller, a heating mantle, and a syringe pump fitted with a Teflon needle. The flask was vented to a water trap for collection of by-product hydrogen bromide. Dry bromine (3410.1 grams, 21.34 moles, 1000% excess) was charged into the reaction flask, followed by 6.5 grams of aluminum chloride (0.049 mole). The reaction was stirred for five minutes.Addition of 33.0 grams (0.19 mole) of diphenyl ether was initiated to the bromine-catalyst mixture at a temperature of 25 C. The diphenyl ether addition was maintained at a constant rate by use of a syringe pump over a period of about 60 minutes. The reaction temperature was allowed to increase by way of exotherm to about 31 C. Additional heat was applied after the diphenyl ether addition had been completed, and the reaction temperature increased to about 59 C. within about 20 minutes. After about 24 hours of post…

The synthetic route of 101-84-8 has been constantly updated, and we look forward to future research findings.