Month: September 2021

Adding a certain compound to certain chemical reactions, such as: 60876-70-2, name is 1-Bromo-4-(tert-butoxy)benzene, 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 60876-70-2, category: ethers-buliding-blocks

Compound (T-22) (179.7 g, 784.5 mmol), bispinacolato diborane (239.0 g, 941.4 mmol), potassium acetate (92.4 g, 941.4 mmol), bis(diphenylphosphino ferrocene dichloropalladium(II) (10.0 g, 13.7 mmol) and 1,3-dioxane (1,000 mL) were mixed, and the resulting mixture was stirred at 90 C. for 4 hours. The reaction mixture was allowed to cool to room temperature, and then poured into water, and subjected to extraction with heptane (800 mL). The extracted layer was washed with water (1,000 mL) and saturated brine (500 mL), dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography (eluent:heptane) to obtain compound (T-23) (182 g, 659 mmol, 84.10).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; JNC Co., Ltd.; JNC Petrochemical Co., Ltd.; Kobayashi, Masahide; Goto, Yasuyuki; Goto, Mayumi; (103 pag.)KR2016/2826; (2016); A;,
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366-99-4, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 366-99-4 name is 3-Fluoro-4-methoxyaniline, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Example 18 Synthesis of (4-Chloro-6-cyclohexylmethoxy-[1,3,5]triazin-2-yl)-(3-fluoro-4-methoxy-phenyl)-amine (114) To a sample of 113 (1.011 g, 3.8 mmol) dissolved in acetone (20 mL) was added a solution of 3-fluoro-p-anisidine (0.541 g, 3.8 mmol) in acetone (10 mL) followed by addition of NaOH (1.52 mL, 2.5 N, 3.8 mmol) and water (3 mL). The reaction mixture was allowed to stir at reflux for about 3 hours under nitrogen. The reaction mixture was extracted 3 times with dichloromethane; the combined organic layers were washed with brine solution and dried over potassium carbonate. The sample was concentrated on a rotary evaporator and the resulting oil was dried overnight under vacuum. Column chromatography (silica gel, 70:30 hexanes:ethyl acetate) yielded light yellow solid compound 114 (0.581 g, 42percent), mp 98° C.; TLC (silica gel, 30:70 ethyl acetate:hexanes), Rf 0.36; MS (ESI): m/z 369 (39.1), 368 (22.1), 367 (M+H, 100), 273 (3.2), 271 (10.7). Example 19 Synthesis of 6-Cyclohexylmethoxy-N,N’-bis-(3-fluoro-4-methoxy-phenyl)-1,3,5-triazine-2,4-diamine (115) [0741] Compound 115 was obtained as a by-product (0.159 g) via column chromatography (silica gel, 70:30 hexanes:ethyl acetate), mp 181° C.; TLC (silica gel, 30:70 ethyl acetate:hexanes), Rf 0.17; MS (ESI): m/z 472 (M+H, 100), 261 (1.5).

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; Timmer, Richard T.; Alexander, Christopher W.; Pillarisetti, Sivaram; Saxena, Uday; Yeleswarapu, Koteswar Rao; Pal, Manojit; Reddy, Jangalgar Tirupathy; Krlshna Reddy, Velagala Venkata Rama Murali; Sridevi, Bhatlapenumarthy Sesha; Kumar, Potlapally Rajender; Reddy, Gaddam Om; US2004/209880; (2004); A1;,
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Reference of 1978-39-8, The chemical industry reduces the impact on the environment during synthesis 1978-39-8, name is 5-Fluoro-2-methoxyaniline, I believe this compound will play a more active role in future production and life.

Step (c): Preparation of 1-(3-fluoro-6-methoxyphenyl)piperazine 5-fluoro-2-methoxyaniline (0.092 mol) and bis(2-chloroethyl)aminehydrochloride (0.1 mol) in xylene (300 ml) was refluxed with stirring for a period of 20 hrs. Water was added to the reaction and the organic layer discarded. The aqueous layer was basified with sodium hydroxide and extracted with methylene chloride (2*100 ml). The methylene chloride extract was dried (sodium carbonate), filtered, and concentrated. Residual material was distilled to provide 8.8 g (45% yield) of piperazine product, b.p. 111-114 C. 0.15 mmHg:

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, 5-Fluoro-2-methoxyaniline, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Bristol-Myers Company; US4585773; (1986); A;,
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Electric Literature of 1077-01-6, A common heterocyclic compound, 1077-01-6, name is 1-Fluoro-3-(trifluoromethoxy)benzene, molecular formula is C7H4F4O, 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.

Under ice cooling mixture of 3-fluoro – trifluoromethoxyphenyl (20g) was dissolved in 40 ml of concentrated sulfuric acid, with rapid stirringWas added portionwise potassium nitrate (28g), was stirred at 0oC 3 hours and stirred at room temperature overnight, the reaction solution was carefullyGo on into 1 kg ice, stirred for 30 minutes, extracted with ethyl acetate, dried over sodium sulfate, filtered, and the filtrate was evaporated, the residue was purified by column chromatography to give 12 g pale yellow 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; Shanghai Hansen Biological Pharmaceutical Co., Ltd.; Jiangsu Stockhausen Pharmaceutical Group Co., Ltd.; Sun, Xingyi; Wei, Mingsong; Cui, Yuanyuan; Tong, Chaolong; Zhang, Fujun; Bao, Rudi; Yu, Hongping; Xu, Yaochang; (41 pag.)CN105503827; (2016); A;,
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Some common heterocyclic compound, 7252-83-7, name is 2-Bromo-1,1-dimethoxyethane, molecular formula is C4H9BrO2, 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. SDS of cas: 7252-83-7

[000321] A mixture of 4-chlorophenol (10 g, 78 mmol), 2-bromo-l,l- dimethoxyethane(13.1 g, 78 mmol), K2C03 (14 g, 101 mmol), KI (100 mg) in DMF (50 mL) was stirred at reflux for 3 h. The mixture was cooled to rt and filtered. The filtrate was added water (200 mL), extracted with ethyl acetate (100 mL x 2), washed with water (100 mL x 3), brine (100 mL x 1), dried over Na2S04, concentrated, and purified by column chromatography on silica gel (ethyl acetate in petroleum ether, 10% v/v) to yield Compound 11A (15 g, yield 89 %) as a colorless liquid. 1H-NMR (CDC13, 400 MHz) major characteristic peaks: delta (ppm) 3.45 (s, 6H), 3.96 (d, J= 5.2 Hz, 2H), 4.70 (t, J= 5.6 Hz, 1H), 6.85 (d, J= 8.8 Hz, 2H), 7.21 (d, J= 8.8 Hz, 2H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 7252-83-7, its application will become more common.

Reference:
Patent; BIOMARIN PHARMACEUTICAL INC.; WANG, Bing; CHU, Daniel; BRIDGES, Alexander, James; WO2015/42397; (2015); A1;,
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Adding a certain compound to certain chemical reactions, such as: 16728-64-6, name is 3-(Benzyloxy)propan-1-amine, 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 16728-64-6, Computed Properties of C10H15NO

Step 3 3-(3-(benzyloxy)propyl)-6-methoxyquinazoline-2,4(1H,3H)-dione To a solution of 6-methoxy-1H-benzo[d][1,3]oxazine-2,4-dione (0.92 g, 4.77 mmol) in THF (10 mL) was added 3-(benzyloxy)propan-l-amine (0.94 g, 5.72 mmol) and then TEA (0.97 g, 9.54 mmol) dropwise. The reaction was heated at 80C for lh, cooled to RT and diluted with EA (20 mL) and water (10 mL). The organic layer was dried over Na2SC>4 and concentrated to a brown oil. The oil was dissolved in THF (10 mL), cooled to 0C, then triphosgene (565 mg, 1.91 mmol) was added. The reaction was stirred at RT for 30 min then TEA (389 mg, 3.82 mmol) was added. The reaction was stirred at RT for 2h and filtered. The filtrate was concentrated and dried to give 3-(3-(benzyloxy)propyl)-6-methoxyquinazoline-2,4(1H,3H)-dione (1.3 g, 80% yield) as a brown oil. LCMS: MH 341 and TR = 1.456 min. Used without further purification.

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, 3-(Benzyloxy)propan-1-amine, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; HYDRA BIOSCIENCES, INC.; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; CHENARD, Bertrand L.; GALLASCHUN, Randall J.; (73 pag.)WO2016/23826; (2016); A1;,
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Electric Literature of 20781-20-8, 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. 20781-20-8, name is (2,4-Dimethoxyphenyl)methanamine belongs to ethers-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Add methyl 2-[(£’)-2-(dimethylamino)vinyl]-5-nitro-benzoate (2.4 Kg crude, 9.65 mol), 2,4-dimethoxybenzylamine (2.14 Kg, 12.8 mol) and toluene (30 L). Heat the mixture to 95-100 C and stir at that temperature for 16 hours. Cool to 20-25 C and collect the precipitated solid by filtration. Dry the yellow solid in the air for two days to give the crude product (2.17 Kg, 66%) which is used without further purification. ES/MS (m/z): 341.1 (M+H).

The synthetic route of (2,4-Dimethoxyphenyl)methanamine has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ELI LILLY AND COMPANY; BROOKS, Harold Burns; DALLY, Robert Dean; DURHAM, Timothy Barrett; FALES, Kevin Robert; FRIMPONG, Kwame; MCCOWAN, Jefferson Ray; NJOROGE, Frank George; SHEPHERD, Timothy Alan; SI, Chong; THRASHER, Kenneth Jeff; TOTH, James Lee; WU, Zhipei; (106 pag.)WO2016/89670; (2016); 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. 7664-66-6, name is 4-Isopropoxyaniline, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of 4-Isopropoxyaniline

General procedure: N,N’-di(2-fluorophenyl)-4-methoxyl-isophthalamide(1a): Equipped a stirrer in a three-necked flask (100 ml), to a mixture of 2-fluoroaniline (1.11 g, 10.0 mmol),anhydrous tetrahydrofuran (15 ml) and dry pyridine (1 ml), dropwise added 4-methoxyl-isophthaloyl dichloride (1.17 g, 5.0 mmol) which had been dissolved in dry tetrahydrofuran (10 ml). After the mixture reaction at room temperature for 8 h under continuous stirring, the excess tetrahydrofuran was distilled off in vacuum. The residue was recrystallized by acetone. Its melting point is 204-206 C, and yield is 67%. The other compounds 1b-1j, 2a-2k, 3a-3l and 4a-4h were prepared in the same manner.

According to the analysis of related databases, 7664-66-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Liu, Xiu Jie; Shi, Xin Xin; Zhong, Yong Liang; Liu, Ning; Liu, Kai; Bioorganic and medicinal chemistry letters; vol. 22; 21; (2012); p. 6591 – 6595,5;,
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Related Products of 22483-09-6, The chemical industry reduces the impact on the environment during synthesis 22483-09-6, name is 2,2-Dimethoxyethanamine, I believe this compound will play a more active role in future production and life.

Compound 3 (1.0 g, 6.82 mmol) was dissolved in aqueous NaOH (0.275 g in 20 ml water) to yield a clear solution. Aminoacetaldehyde dimethyl acetal (0.93 ml, 8.58 mmol) was added. The mixture was placed on an oil bath (120-130 C); foaming lasted for 3 h. The mixture was cooled. The resulting grey powder was recovered by filtration, washed with cold water, and dried under high vacuum to give 4 (yield 1.3 g, 88%). 1H NMR (D2O): 2.79 (s, 2H), 2.81 (s, 6H), 3.99 (t, J =5.4 Hz, 1H).

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, 2,2-Dimethoxyethanamine, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Laos, Roberto; Lampropoulos, Christos; Benner, Steven A.; Acta Crystallographica Section C: Structural Chemistry; vol. 75; 1; (2019); p. 22 – 28;,
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