Synthetic Route of 454-31-9,Some common heterocyclic compound, 454-31-9, name is Ethyl 2,2-difluoroacetate, molecular formula is C4H6F2O2, 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.
109 g (0.88 mol) of ethyl alpha, alpha-difluoroacetate was added to a stainless steel pressure-proof reaction vessel,0.107 g (0.18 mmol) of a ruthenium catalyst represented by the following formula42 g of sodium methoxide 28% methanol solution (0.22 mol of sodium methoxide)Methanol 290mL,The reactor was replaced with hydrogen 5 times,The hydrogen pressure was set to 1.0 MPa,After stirring at 15 C for 8 hours,React.After 19F-NMR analysis of the reaction, the conversion of alpha, alpha-difluoroacetic acid ethyl ester was 65%, and the selection of DFAL-EtOHThe rate is 91%. 19F-NMR was quantified with the internal standard substance alpha, alpha, alpha-trifluorotoluene.To the reaction solution was added 13.2 g (0.22 mol) of acetic acid,Then adjusting the pH to 8, judging that it is substantially neutral,Abort add.The liquid was directly distilled (bottom temperature ~ 66 C,Decompression degree ~ 2.1 kPa) to obtain a methanol solution containing DFAL-EtOH.The solution was distilled (theoretical plates 35 plates,Distillation temperature 92 ,Decompression degree ~ 35kPa) Most of the methanol separation.To a still pot (bottom) were added 96 g (2.08 mol) of ethanol,Continue distillation,45.9 g of DFAL-EtOH was obtained as a fraction.
The synthetic route of 454-31-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Center Xiaozi Co., Ltd.; Mu Cunzhenren; Qiu Yejinye; Wu Tianjiangzhang; Tian Zhongyishu; Teng Benyalong; (13 pag.)CN107438592; (2017); A;,
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