Month: July 2021

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 31804-36-1 as follows. Recommanded Product: 1-Bromo-3-methoxy-2-methylbenzene

A solution of 7g3, (9.3 g, 46 mmol), N-bromosuccinimide (8.2 g, 46 mmol) and benzoyl peroxide (450 mg, 1.8 mmol) in CCI4 (100 mL) is heated to reflux and stirred for 6 h. The reaction mixture is cooled to RT, and then filtered. The filtrate is diluted with DCM and washed successively with 2.0 N NaOH, water and brine. The organic layer is dried over MgS04, filtered and concentrated under vacuum to give 7g4.

According to the analysis of related databases, 31804-36-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; SIMONEAU, Bruno; DEROY, Patrick; FADER, Lee; FAUCHER, Anne-Marie; GAGNON, Alexandre; GRAND-MAITRE, Chantal; KAWAI, Steven; LANDRY, Serge; MERCIER, Jean-Francois; RANCOURT, Jean; WO2011/100838; (2011); 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. 588-63-6, name is (3-Bromopropoxy)benzene, A new synthetic method of this compound is introduced below., name: (3-Bromopropoxy)benzene

The 148mg Na dissolved in 20ml of absolute ethanol until complete dissolution, 6-benzyl-2-thiouracil200mg (0.92mmol) and 1-(3-bromopropoxy)benzene 297mg (1.38mmol) was added, at room temperature after stirring overnight the reaction was complete by TLC; column chromatography, P:E = 5:1,2:1,1:1, finally give 257 mg of the product, as a white solid, a yield of 79.17percent

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; Peking University; Zhang, Liang; FU, YUHONG; Qin, Hua; Wang, Xiao Wei; Liu, Jun Yi; (30 pag.)CN103864699; (2016); B;,
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. 1663-61-2, name is (Triethoxymethyl)benzene, A new synthetic method of this compound is introduced below., Recommanded Product: 1663-61-2

Phenyltriethoxymethane (0.5 mL) and acetic anhydride (0.94 mL) were added to malononitrile (0.17 g), and the mixture was stirred at 140 ° C. overnight.After the reaction solution was cooled to room temperature, the solvent was distilled off under reduced pressure to obtain a crude product.Purification by silica gel column chromatography (ethyl acetate – hexane)2- (Ethoxy (phenyl) methylene) malononitrile(Compound 0022-1, 334 mg) was obtained

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; FUJIFILM CORPORATION; KYOTO UNIVERSITY; KATO, TAKAYUKI; HIRAI, ATSUSHI; MATSUOKA, MASAO; SHIMURA, KAZUYA; (62 pag.)JP6052673; (2016); B2;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Related Products of 24988-36-1, 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. 24988-36-1, name is 1,5-Dibromo-2,4-dimethoxybenzene, This compound has unique chemical properties. The synthetic route is as follows.

(B-1) Synthesis of 2,4-bis(2-fluorophenyl)-1,5-dimethoxybenzene 2,4-dibromo-1,5-dimethoxybenzene (88.8g, 300 mmol, 1eq.), 2-fluorophenylboronic acid (100.74g, 720 mmol, 2.4 eq.), Na2CO3 2M aq. (600 mL), Pd(PPh3)4 (6.73g, 6 mmol, 2 mol%), 1,2-dimethoxyethane (150 mL) and toluene (150 mL) were placed in a flask, and the resulting mixture was refluxed for 36 hours. After completion of the reaction, water (500 mL) and toluene (1 L) were added, and the mixture was transferred to a separating funnel, whereby a toluene phase was collected. After drying with MgSO4, original impurities were removed by passing through, a silica gel short column, thereby to concentrate the solution. The thus concentrated solution was recrystallized from a toluene/hexane mixed solvent, whereby white crystals of 86.5g (yield: 88%) of 2,4-bis(2-fluorophenyl)-1,5-dimethoxybenzene were obtained.

The chemical industry reduces the impact on the environment during synthesis 1,5-Dibromo-2,4-dimethoxybenzene. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Idemitsu Kosan Co., Ltd.; EP2436679; (2012); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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. 4342-46-5, name is 4-Methoxycyclohexanamine, This compound has unique chemical properties. The synthetic route is as follows., category: ethers-buliding-blocks

1200 mL of water was added to the autoclave.Turn on stirring,Add 40% Formamide 220g (2mol), After stirring for 10 minutes,1-amino-4-methoxycyclohexane 130 g (1 mol) was added,Then add ruthenium carbon catalyst 7g,Pass CO into the reactor,The pressure in the kettle reaches 0.2MPa,Raise the temperature to 50CInsulation 20hControl raw materials < 2%,The reaction is over,Cool down to 2530C,Dilute hydrochloric acid was added dropwise to the reaction solution.Adjust the pH to 5-6.There is a solid precipitated,Filter out products,The cake is shuffled onceObtained 169 g of cis-8-methoxy-1,3-diazaspiro[4,5]-indol-2,4-dione as a dry product.Yield 84.5%; According to the analysis of related databases, 4342-46-5, the application of this compound in the production field has become more and more popular. Reference:
Patent; Henan Longhu Biological Co., Ltd.; Mu Kairui; Guo Shuai; Xu Caiyun; (11 pag.)CN107721996; (2018); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Reference of 1579-40-4, A common heterocyclic compound, 1579-40-4, name is Di-p-tolyl Ether, molecular formula is C14H14O, 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: To the 250 mL 3-neck RB flask charged di-p-tolylether (10 g, 50.43 mmol), benzoicacid (7.39 g, 60.52 mmol) and ZnCl2 (19.73 g, 144.73 mmol) in POCl3 (15 mL)and stirred mechanically for few minutes. Then the reaction mixture heated up to95C and allowed to stir for 4h. After 4h, color of the reaction mixture turned intodark brown and unable to stir. Then the above reaction mixture cooled to 0C andquenched with crushed ice (40 g) while mechanically stirring. To the above reactionmixture added H2O (150 ml) and allowed to stir at RT for 16h.The obtainedsolid suspension filtered through Buchner funnel and the solid cake washed withH2O (3 × 50 mL) followed by hexane (2 × 100 mL) to get crude DMPx-OH. Thiscrude solid re-dissolved in EtOAc (200 mL) and taken into separating flask andwashed with sat NaHCO3 (2 × 50 mL), the organic layer dried over Na2SO4 andevaporated the solvent on rotary evaporator to get off-white color DMPx-OH 2(10.37 g, 68%).1H NMR (400 MHz, CDCl3) delta: 2.24 (s, 6H), 2.55 (s, 1H), 7.07 (m, 4H), 7.12 (t, J= 0.8 Hz, 2H), 7.19 (m, 1H), 7.29 (m, 2H), 7.40 (dd, J1 = 8.3, 1.1 Hz, 2H).MS: 285.6 (M +).

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:
Article; Penjarla, Srishylam; Prasad, S. Rajendra; Reddy, Dhande Sudhakar; Banerjee, Shyamapada; Penta, Santhosh; Sanghvi, Yogesh S.; Nucleosides, nucleotides and nucleic acids; vol. 37; 4; (2018); p. 232 – 247;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Some common heterocyclic compound, 54314-84-0, name is ((3-Bromopropoxy)methyl)benzene, molecular formula is C10H13BrO, 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. HPLC of Formula: C10H13BrO

Example 7.9 Preparation of (1S,5R,6R)-3-(3-(benzyloxy)propyl)-10-((3,5-dichlorophenyl)sulfonyl)-5-vinyl-3,10-diazabicyclo[4.3.1]decan-2-one J1 To a solution of (1S,5R,6R)-10-((3,5-dichlorophenyl)sulfonyl)-5-vinyl-3,10 – diazabicyclo [4.3.1] decan-2-one (35.0 mg, 0.0899 mmol) in DMF (1.0 mL) was added NaH (5.39 mg, 0.135 mmol). After 20 minutes ((3-bromopropoxy)methyl)benzene (20.6 mg, 0.0899 mmol) was added, the solution was heated to 80 °C and stirred for 1 h. Et2O (90 mL) was added to the solution and washed with sat. aq. NaCl solution (3 * 10 mL). The organic layer was dried over MgSO4 and the solvent removed under reduced pressure. Column chromatography on SiO2 (Cyclohexane/EtOAc = 1:1) afforded the title compound (31.0 mg, 0.0577 mmol, 64.2 percent) as a colorless solid. Rf: 0.25 (Cyclohexane/EtOAc = 7:3) 1H NMR (600 MHz, CDCl3) delta = 1.28 (s, 2 H), 1.47 – 1.54 (m, 3 H), 1.83 – 1.92 (m, 2 H), 2.23 – 2.29 (m, 1 H), 2.58 – 2.64 (m, 1 H), 2.95 – 3.00 (m, 1 H), 3.49 – 3.59 (m, 4 H), 3.95 – 4.04 (m, 2 H), 4.50 (s, 2 H), 4.65 (d, J = 6.2 Hz, 1 H), 5.09 – 5.15 (m, 2 H), 5.74 – 5.82 (m, 1 H), 7.28 (s, 1 H), 7.33 (d, J = 1.3 Hz, 4 H), 7.56 (s, 1 H), 7.69 (d, J =1.8Hz,2H). 13C NMR (150 MHz, CDCl3) delta = 15.42, 26.29, 26.89, 27.36, 28.14, 29.68, 49.16, 49.53, 51.85, 54.83, 56.84, 67.64, 73.08, 116.8, 124.9, 127.6, 127.7, 128.4, 132.6, 136.3, 137.2, 138.2, 144.1, 169.7.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 54314-84-0, its application will become more common.

Reference:
Patent; Max-Planck-Gesellschaft zur Foerderung der Wissenschaften e.V.; The designation of the inventor has not yet been filed; EP2899192; (2015); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Synthetic Route of 64465-53-8, 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. 64465-53-8, name is 4-Fluoro-3-methoxyaniline, This compound has unique chemical properties. The synthetic route is as follows.

Example 1; 4-Bromo- 1 -fluoro-2-methoxybenzene; Aqueous hydrobromic acid (48%, 2.41 mL) was added to 4-fluoro-3-methoxyaniline (1.0 g, 7.1 mmol) in water (10 mL) and the resulting mixture was cooled to 0 0C in an ice bath. A solution of sodium nitrite (538 mg, 7.8 mmol) in water (5 mL) was added drop wise during 15 min while maintaining the temperature between 0-5 0C. The resulting diazoniumsalt solution was added to a suspension of copper (I) bromide (1.12 g, 7.8 mmol) in water (5 mL) which had been pre-heated to 75 C. The mixture was shaken thoroughly, aqueous hydrobromic acid (48%, 12.07 mL) was added and the solution was stirred at ambient temperature for 16 h. Excess water was added and the product was extracted with diethyl ether and the combined organic extracts were washed with aqueous saturated sodium chloride, dried over magnesium sulfate, filtered and the solvent was evaporated in vacuo to give 1.02 g (70% yield) of the title compound: 1H-NMR (DMSO-afo): delta 7.36 (dd, J = 7.78, 2.26 Hz, 1 H), 7.23 – 7.17 (m, 1 H), 7.14 – 7.09 (m, 1 H), 3.86 (s, 3 H); MS (EI) m/z 204, 206 [M+«]

The chemical industry reduces the impact on the environment during synthesis 4-Fluoro-3-methoxyaniline. I believe this compound will play a more active role in future production and life.

Reference:
Patent; ASTRAZENECA AB; ASTEX THERAPEUTICS LTD; WO2007/145568; (2007); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Synthetic Route of 437-82-1, A common heterocyclic compound, 437-82-1, name is 2,6-Difluoroanisole, molecular formula is C7H6F2O, 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.

5 g (34.7 mmol) of 2,6-difluoroanisole and 2.62 g (40 mmol) of cyclopropylnitrile are added in 100 ml of toluene. At room temperature, 77 ml of a 0.5 M solution of KHMDS in toluene is added in drops. The reaction mixture is heated slightly. After stirring overnight at room temperature, water and ethyl acetate are added. It is shaken with 10% sulfuric acid, and the organic phase is separated. After repeated shaking of the aqueous phase with ethyl acetate, the combined organic extracts are washed with brine. After drying on sodium sulfate, it is filtered off, and the solvent is spun off. After chromatography on silica gel (mobile solvent: ethyl acetate/hexane), 2.53 g (38.2%) of the desired compound is obtained.

The synthetic route of 437-82-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Schmees, Norbert; Lehmann, Manfred; Rehwinkel, Hartmut; Strehike, Peter; Jaroch, Stefan; Schaecke, Heike; Schottelius, Amdt J.G.; US2004/209875; (2004); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

These common heterocyclic compound, 29578-39-0, name is 1-Bromo-3-fluoro-5-methoxybenzene, 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. Computed Properties of C7H6BrFO

(Example 40) 3-{[6-(3-Fluoro-5-methylphenoxy)-1-methyl-1H-benzimidazol-2-yl]methoxy}benzoic acid (Compound No. 1-188) (40a) 1-Fluoro-3-methoxy-5-methylbenzene A mixed solution of 3-bromo-5-fluoroanisole (2.05 g, 10 mmol), trimethylboroxine (50% solution in THF, 2.51 g, 20 mmol), PdCl2(dppf) (0.82 g, 1.0 mmol) and cesium carbonate (6.52 g, 20 mmol) in dioxane (100 mL) and water (50 mL) was stirred with heating under reflux for 10 hours. After leaving to cool, water (100 mL) was added to the reaction solution, followed by extraction with ethyl acetate (200 mL) twice. The organic layers were washed with water (100 mL) twice and dried over anhydrous sodium sulfate. After concentration under reduced pressure, the residue was purified by silica gel chromatography (hexane:ethyl acetate, 6:1) to obtain the title compound (1.40 g, yield: 66%) as a yellow oil. 1H-NMR (CDCl3, 400 MHz) delta: 1.78 (3H, s), 6.44 (1H, dd, J = 2.0, 11.0 Hz), 6.50 (1H, d, J = 11.0 Hz), 6.51 (1H, s).

The synthetic route of 1-Bromo-3-fluoro-5-methoxybenzene has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Daiichi Sankyo Company, Limited; EP2138484; (2009); A1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem