Category: 1188911-72-9

Reference of 1188911-72-9, These common heterocyclic compound, 1188911-72-9, name is Methyl 3,3,3-trifluoro-2,2-dimethylpropanoate, 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.

To a mixture of acetonitrile (3.32 mL, 97 mmol) in THF (300 mL) cooled to -78 C. was added n-BuLi (56.4 mL, 141 mmol).The mixture was stirred at -30 C. for 30 min. Then to the mixture was added methyl 3,3,3-trifluoro-2,2-dimethylpropanoate (15 g, 88 mmol) dropwise. The mixture was stirred at 25 C. for 10 h. The mixture was quenched with NH4Cl (aq) and extracted with DCM/MeOH (10:1). The organic layer was dried over Na2SO4, filtered and concentrated. The crude material was purified by silica column chromatography (PE/EA=10:1). All fractions found to contain product by TLC (PE/EA=5:1, Rf=0.6) were combined and concentrated to yield a light yellow solid of 5,5,5-trifluoro-4,4-dimethyl-3-oxopentanenitrile (5 g, 27.9 mmol, 31.7% yield): 1H NMR (400 MHz, CDCl3) delta: 3.75 (s, 2H), 1.41 (s, 6H).

Statistics shows that Methyl 3,3,3-trifluoro-2,2-dimethylpropanoate is playing an increasingly important role. we look forward to future research findings about 1188911-72-9.

Reference:
Patent; GlaxoSmithKline Intellectual Property Development Limited; EIDAM, Hilary Schenck; Raha, Kaushik; Gong, Zhen; Guan, Huiping; Wu, Chengde; Yang, Haiying; Yu, Haiyu; Zhang, Zhiliu; CHEUNG, Mui; US2014/275111; (2014); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

These common heterocyclic compound, 1188911-72-9, name is Methyl 3,3,3-trifluoro-2,2-dimethylpropanoate, 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. Quality Control of Methyl 3,3,3-trifluoro-2,2-dimethylpropanoate

[00444] To a -78 C solution of diisopropylamine (15 mL, 107 mmol) in THF (150 mL) was added n-BuLi (2.4 mol/L, 8 mL) dropwise. The reaction mixture was stirred for 30 minutes and a solution of methyl 3,3,3-trifluoro-2,2-dimethylpropanoate (3 g, 17.63 mmol) in acetonitrile (10 mL, 239 mmol) was added dropwise slowly. One hour later, the mixture was warmed slowly to rt and stirred for 2 hours. The mixture was quenched with saturated aqueous ammonium chloride solution (50 mL), and the resulting mixture was extracted with ethyl acetate (300 mL), dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated in vacuo and the residue was purified by silica gel column chromatography (EtOAc/PE (v/v) = 1/1) to give the title compound as a white solid (1.53 g, 48%). The compound was characterized by the following spectroscopic data: MS-ESI: (ESI, pos.ion) m/z: 180.1 [M+lfb; and ?H NMR (600 MHz, CDC13) 3.77 (s, 2H), 1.43 (s, 6H).-78 C

The synthetic route of Methyl 3,3,3-trifluoro-2,2-dimethylpropanoate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SUNSHINE LAKE PHARMA CO., LTD.; CHENG, Changchung; ZHANG, Yingjun; LIU, Bing; LONG, Bohua; CHEN, Yu; CHENG, Zhixin; (182 pag.)WO2016/8433; (2016); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics