Synthetic Route of 60758-86-3,Some common heterocyclic compound, 60758-86-3, name is 3-Ethoxy-4-methoxybenzonitrile, molecular formula is C10H11NO2, 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.
The reaction flask was charged with 400 mL of tetrahydrofuran and 62.5 g (0.8 mol) of dimethylsulfoxide,Stirring to cool to 0 C to 5 C,500 mL (0.8 mol) of a 1.6 M n-butyllithium n-hexane solution having the same temperature of 0 C. to 5 C. was added, and the mixture was stirred for 1.5 hours.Another 179.0 g (0.55 mol) of tributyltin chloride in 450 mL of tetrahydrofuran was added And 88.6 g (0.5 mol) of 3-ethoxy-4-methoxybenzonitrile (Formula III),Stirred for 0.5 hours, naturally warmed to 15 C to 20 C for 2 hours,1000mL purified water was added and the reaction was continued at 15 C to 20 C for 12 hours.The reaction was stopped, the solid obtained in the reaction solution was filtered, and the filter cake was washed with 100 mL each of purified water, n-hexane and tetrahydrofuran in that order. After drying to give a white solid 109.6g, calculated according to the molar yield of Compound III 85.2%, HPLC The degree is 98.1% and the ee is 97.3%.
The synthetic route of 60758-86-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Peking University Fangzheng Group Co., Ltd.; Chongqing Southwest Synthetic Pharmaceutical Co., Ltd.; Peking University Medical Treatment Industrial Group Co., Ltd.; Fu Biao; Zou Aifang; Luo Li; (9 pag.)CN106866475; (2017); A;,
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