Electric Literature of 243128-37-2, A common heterocyclic compound, 243128-37-2, name is 4-Fluoro-3-methoxybenzonitrile, molecular formula is C8H6FNO, 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.
Add lithium chloride (1.7 g, 40 mmol) to a stirred solution of 4-fluoro-3- methoxybenzonitrile (2.0 g, 13 mmol) in DMF (26 mL). Stir the resulting mixture at 160 C for 5 hours and then cool to room temperature with stirring for 12 hours. Dilute the mixture with ethyl acetate (50 mL) and wash with water (2 x 40 mL). Acidify the isolated aqueous phase with 1 M HC1 and extract with ethyl acetate (3 x 60 mL). Wash the combined organic extracts with water (2 x 100 mL), dry over Na2SC”4, and concentrate under reduced pressure to give the title compound as a yellow solid (0.68 g, 38%): ES/MS (m/z) 138 (M+H), which is directly used without further purification.
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; ELI LILLY AND COMPANY; LILLY CHINA RESEARCH AND DEVELOPMENT CO., LTD.; LIU, Kevin Kun-Chin; XIE, Yinong; WU, Liang; ZHOU, Guoqiang; WO2015/89800; (2015); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts