Ethers-buliding-blocks

Synthetic Route of 2062-98-8, 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. 2062-98-8, name is Perfluoro(2-methyl-3-oxahexanoyl) fluoride belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example 2; Example 2-1; [0175] Example for Preparation of CH2CHCH(OCH3) CH2OCOCF (CF3)OCF2CF2CF3; [0176] CH2CHCH(OCH3)CH2OH (270 g) was charged together with NaF (334 g) into a 2 L pressure resistant reactor equipped with a reflux condenser in which a coolant at 20 C. circulated, and stirred at -10 C. While discharging by-product HF formed by the reaction out of the system from the reflux condenser on the upper portion by bubbling nitrogen gas to the reactor, FCOCF(CF3)OCF2CF2CF3 (1055 g) was dropwise added over a period of 1.5 hours. At this time, the temperature was adjusted so that the internal temperature of the reactor would be at most 0 C. After completion of the dropwise addition, stirring was carried out at 30 C. for 18 hours and then the reaction was terminated. [0177] NaF contained in the crude liquid after completion of the reaction was collected by filtration to obtain a crude product (981 g) (yield 86.4%). As a result of the analysis by NMR, the above-identified mixture was obtained as a liquid mixture with FCOCF(CF3)OCF2CF2CF3. The results of analysis of the above-identified compound are as follows. [0178] 1H-NMR(300.4 MHz, solvent:CDl3, standard:TMS) delta (ppm):3.29(s, 3H), 3.85-3.90(m, 1H), 4.24-4.45(m, 2H), 5.34(s, 1H), 5.39(d,J=8.4 Hz, 1H), 5.59-5.71(m, 1H). [0179] 19F-NMR(282.7 MHz, solvent:CDCl3, standard:CFCl3) delta (ppm): -81. 8(3F), -82.6(3F), -79.9-87.5(2F), -130.2(2F), -132.3(1F).

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, Perfluoro(2-methyl-3-oxahexanoyl) fluoride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; ASAHI GLASS COMPANY LIMITED; US2003/216595; (2003); A1;,
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Synthetic Route of 22483-09-6, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 22483-09-6 as follows.

A solution of aminoacetaldehyde dimethyl acetal (25 mL, 229 mmol) in toluene (120 mL) is treated at 0 C with a 4.85 M sodium hydroxide solution (70.8 mL, 343.5 mmol). The mixture is stirred at 0 C for 10 minutes and benzyl chloroformate (33.8 mL, 229 mmol) is added keeping the internal temperature below 20 C during the addition. The mixture is warmed to room temperature over 4 hours. The organic layer is separated, washed with brine, dried over sodium sulfate, and concentrated to dryness to give the title compound (54 g, 98 %). ES/MS (m/e): 240 (M+H).

According to the analysis of related databases, 22483-09-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ELI LILLY AND COMPANY; GREEN, Steven James; MERGOTT, Dustin James; WATSON, Brian Morgan; WINNEROSKI JR., Leonard Larry; WO2014/143579; (2014); A1;,
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Synthetic Route of 6346-09-4, A common heterocyclic compound, 6346-09-4, name is 4,4-Diethoxybutan-1-amine, molecular formula is C8H19NO2, 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.

Step1 To the stirred solution of 1,3-dioxo-1,3-dihydro-isoindole-2-carboxylic acid ethyl ester (10 g, 62 mmol, 1 eq) in dry THF (200 mL) were added 4,4-diethoxy-butylamine (13.6 g, 62 mmol, 1 eq) and TEA (8.6 mL, 62 mmol, 1 eq) under ice cooled condition and stirred at RT for 16 h. After completion of the reaction, it was concentrated under reduced pressure to obtain crude product which was purified by silica gel (100-200 mesh) column chromatography (5% EA/Hexane) to afford 2-(4,4-diethoxy-butyl)-isoindole-1,3-dione (17 g, 94% yield) as light yellowish liquid.

The synthetic route of 6346-09-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; GRUeNENTHAL GMBH; JAKOB, FLORIAN; NORDHOFF, SONJA; RIDER, DAVID; WAGENER, MARKUS; BAHRENBERG, GREGOR; DUNKERN, TORSTEN; (70 pag.)US2018/78541; (2018); A1;,
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Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 41365-75-7, name is 1-Amino-3,3-diethoxypropane, This compound has unique chemical properties. The synthetic route is as follows., Safety of 1-Amino-3,3-diethoxypropane

[0080] To a stirred solution of intermediate (9) (287 mmol) in CHCl3 (2000 ml) was added 3,3-diethoxy-1-propanamine (474 mmol) at 0 C. in portions. After the addition, the reaction mixture was stirred at 0 C. for 1 hour and then at 15 C. for 2 hours. Thin Layer Chromatography (petroleum ether/ethyl acetate=5/1) showed that the reaction was completed. The reaction mixture was washed by saturated Na2SO3 aqueous (four times with 600 ml) and then saturated NaHCO3 aqueous was added until pH=7. The aqueous layer was extracted by CH2Cl2 (500 ml). The combined organic phases were washed with brine (800 ml), dried over Na2SO4 and concentrated to give the crude product. The crude product was washed by tert-butyl methylether (three times 500 ml) to give 87 g of intermediate (10) (mp. 100.8-103.8 C.).

According to the analysis of related databases, 41365-75-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ELANCO ANIMAL HEALTH IRELAND LIMITED; Guillemont, Jerome Emile Georges; Raboisson, Pierre Jean-Marie Bernard; Lounis, Nacer; US2013/109694; (2013); A1;,
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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. 2062-98-8, name is Perfluoro(2-methyl-3-oxahexanoyl) fluoride, A new synthetic method of this compound is introduced below., Recommanded Product: 2062-98-8

To a 3 -neck flask equipped with a temperature probe, magnetic stir bar, water- cooled condenser, and addition funnel was charged sodium borohydride (16.0 g, 423 mmol), and tetraethylene glycol dimethyl ether (125 mL). 2,3,3,3-Tetrafluoro-2- (1,1,2,2,3, 3, 3-heptafluoropropoxy)propanoyl fluoride (100 g, 301 mmol) was added dropwise to the resultant mixture. After complete addition, the reaction mixture was heated to reflux and stirred overnight. The mixture was then allowed to cool to room temperature followed by the dropwise addition of methanol (100 mL) and H2O (150 mL). The mixture was then transferred to a separatory funnel and the fluorous phase was collected and then distilled (46.1 C, 40 ton) to afford 2,3,3,3-tetrafluoro-2-(l, 1,2,2,3,3- heptafluoropropoxy)propan-l-ol (67.5 g, 71%) as a colorless liquid. The isolated compound was used in the next step. (0204) To a 3-neck flask equipped with a temperature probe, distillation head, overhead stirrer, and under N2 was charged TiCU (7.9 mL, 72 mmol). 2,3,3,3-Tetrafluoro-2- (l,l,2,2,3,3,3-heptafluoropropoxy)propan-l-ol (15.1 g, 47.8 mmol) was added dropwise with stirring and the resultant mixture was heated to 40 C followed by a 30 min stir. The mixture was then allowed to cool to room temperature followed by the dropwise addition of tetraethylene glycol dimethyl ether (45 mL). Exotherms reaching approximately 50 C were observed. The resultant mixture was allowed to warm to room temperature followed by the addition of zinc dust (9.1 g, 140 mmol) in one portion. The resultant reaction mixture was raised to 85 C. After a 3 h stir, the temperature was slowly raised to 225 C and distillate was collected with the distillation head temperature reaching 69 C affording the title compound (4.1 g, 31%) as a colorless liquid.

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; 3M INNOVATIVE PROPERTIES COMPANY; SMITH, Sean M.; LAMANNA, William M.; COSTELLO, Michael G.; BULINSKI, Michael J.; (35 pag.)WO2017/195070; (2017); A1;,
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In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 36805-97-7 as follows. Quality Control of 1,1-Di-tert-butoxy-N,N-dimethylmethanamine

Step C: (2Z)-1-[2-(3-Bromophenyl)-6-(trifluoromethyl)pyrazolo[1,5-a]pyridin-3-yl]-3-(dimethylamino)-2-fluoro-2-propen-1-one; To a solution of 1-[2-(3-bromophenyl)-6-(trifluoromethyl)pyrazolo[1,5-a]pyridin-3-yl]-2-fluoroethanone (10 mg, 0.025 mmol) in DMF (2 mL) was added DMF di-tert-butyl acetal (0.85 g, 4.2 mmol) and the reaction was heated at 80 C. for 15 min. The crude reaction mixture was adsorbed to silica gel and purified by LC (5-50% EtOAc in hexanes) to give the title compound (10 mg, 88%). ESIMS (M+H)+=456.

According to the analysis of related databases, 36805-97-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; SmithKline Beecham Corporation; US2008/51395; (2008); A1;,
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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. 102503-23-1, name is 1-(2,4-Dimethoxyphenyl)-N-methylmethanamine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 1-(2,4-Dimethoxyphenyl)-N-methylmethanamine

Into a vial was added the [B] 4-bromo-2-fluoro-N-thiazol-2-yl-benzenesulfonamide (170 mg, 0.00050 mol), sodium tert-butoxide (117 mg, 0.00121 mol), 9,9-dimethyl-4,5-bis(diphenylphosphino)xanthene (18 mg, 0.000030 mol), Tris(dibenzylideneacetone)dipalladium(0) (9.3 mg, 0.000010 mol) and 1,4-dioxane (1.58 mL, 0.0202 mol). Argon was bubbled for 15 minutes. Into the reaction was added the [2,4-dimethoxy-benzyl)-methyl-amine (110 mg, 0.00061 mol) and the reaction mixture was heated at 100 C. overnight. The reaction mixture was cooled to room temperature then filtered over Celite. The filtrate was concentrated to give the crude compound as a yellow solid that was used in the next step without purification

The synthetic route of 102503-23-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Icagen; US2009/23740; (2009); A1;,
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Application of 78531-29-0, A common heterocyclic compound, 78531-29-0, name is 1,3-Dimethoxypropan-2-amine, molecular formula is C5H13NO2, 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.

[0407] In Examples, a room temperature usually indicates10 to 30 C. ?H NMR indicates a proton nuclear magnetic resonance spectrum, and chemical shift (6) is expressed in ppm, using tetramethylsilane as an internal standard substance.; [0432] The intermediate compound (1) (0.24 g, 1.0 mmol), 1,3-dimethoxypropane-2-amine (0.15 g, 1.2 mmol), and HOST (0.01 g, 0.1 mmol) were added to chloroform (Amylene-added product) (2.5 mE). Afier EDCD (0.24 g, 1.2 mmol) was added to the mixed liquid at room temperature, the mixture was stirred at room temperature overnight. Thereafier, dilute hydrochloric acid was added to the reaction mixture, followed by extraction with chloroform two times. Afier organic layer was passed through a short column to remove impurities, this was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.26 g of a compound offollowing formula: (hereinafier, referred to as compound (12)).; [0433] ?H-NMR (CDC13, TMS, oe(ppm)): 3.38 (6H, s),3.49-3.53 (2H, m), 3.57-3.61 (2H, m), 4.36-4.43 (1H, m),4.60 (2H, s), 4.65 (2H, s), 6.72 (1H, s), 7.14 (1H, brs),7.30-7.40 (5H, m)

The synthetic route of 78531-29-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SUMITOMO CHEMICAL COMPANY, LIMITED; MITSUDERA, Hiromasa; OKAJIMA, Mayumi; KOWATA, Ayano; AWASAGUCHI, Kenichiro; UJIHARA, Kazuya; (108 pag.)US2017/295789; (2017); A1;,
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Application of 13321-74-9, These common heterocyclic compound, 13321-74-9, name is 4-Bromo-2,5-dimethoxytoluene, 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.

General procedure: A flask containing LiCl (980 mg,23.1 mmol), 2-bromo-4-fluoroanisole (1.0 mL, 7.7 mmol), DCMA (1.8 mL,8.4 mmol) and ethyl 3-ethoxyacrylate (3.3 mL, 23 mmol) in 1,4-dioxane(20 mL) was degassed by passing a stream of nitrogen through the mixturefor 10 min. Bis(tri-t-butylphosphine) palladium(0) (166 mg, 0.32 mmol) wasadded, and reaction mixture was heated at reflux under nitrogen for 16 h. Thebrown mixture was then cooled and partitioned between ethyl acetate andwater. The layers were separated, and the organic layer was washedsequentially with aqueous NH4Cl and brine, followed by drying over Na2SO4.The mixture was filtered, and the filtrate was concentrated under reducedpressure to give an oil which was purified by flash chromatography on silica(40 g, 10-50% ethyl acetate in heptane) to afford 22c as an orange oil (1.93 g,92%) as an inseparable mixture of E- and Z-isomers: 1H NMR (CDCl3, 500 MHz)alkene protons d: 5.21, 5.33 ppm (1:1 ratio); LCMS (ES): 269.2 (MH). HRMSCalcd for C14H17FO: 269.1184. Found: 269.1196.

The synthetic route of 13321-74-9 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Kohrt, Jeffrey T.; Conn, Ed; Maguire, Robert; Wright, Stephen W.; Singer, Robert; Tetrahedron Letters; vol. 54; 51; (2013); p. 7065 – 7068;,
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These common heterocyclic compound, 5414-19-7, name is 1-Bromo-2-(2-bromoethoxy)ethane, 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. COA of Formula: C4H8Br2O

Step a Intermediate 207 -Bromophenyl 2-ethyltetrahydro-2H-pyran-4-carboxylate A mixture of NaH (60% in mineral oil) (2.057 g, 51.4 mmol) in DMF (67 ml) stirred at 0 C was treated dropwise with a mixture of ethyl 2-(4-bromophenyl)acetate (5 g, 20.57 mmol) and 1 -bromo-2-(2-bromoethoxy)ethane (2.59 ml, 20.57 mmol) in 3 ml of diethyl ether. The mixture was allowed to warm to r.t. and stirred for 17 h. Mixture was quenched with water and sat. NH4CI. The mixture was extracted with EtOAc (x 3) and then organics washed with brine (x 3) and dried (MgS04), filtered and concentrated under reduced pressure. The residue was purified by column chromatography (Si02; 0 – 100 % EtOAc in petrol) to yield 4-bromophenyl 2-ethyltetrahydro-2H-pyran-4- carboxylate as a pale yellow oil (2.88 g, 45 %). ? NMR (400 MHz, CD2C12) 57.46 – 7.56 (m, 2H), 7.32 (m, 2H), 4.15 (m, 2H), 3.84 – 3.98 (m, 2H), 3.50 – 3.63 (m, 2H), 2.38 – 2.56 (m, 2H), 1.95 (m, 2H), 1.21 (m, 3H)

The synthetic route of 1-Bromo-2-(2-bromoethoxy)ethane has been constantly updated, and we look forward to future research findings.

Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; RUPRAH, Parminder, Kaur; MERCHANT, Kevin, John; WALSH, Louise, Marie; KERR, Catrina, Morven; FIELDHOUSE, Charlotte; HARRISSON, David; MAINE, Stephanie; HAZEL, Katherine; WO2013/27001; (2013); A1;,
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