HRID1170894

反应详情

EQUATION

反应方程式

HRID 1170894 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred solution of 4-chloro-2-(trifluoromethyl)nicotinic acid (8.75 g, 38.8 mmol) in ethyl acetate (100 mL) in an ice bath is added a solution of diazomethane [generated from 12 g (116 mmol) of N-nitroso-N-methylurea] in diethyl ether (200 mL). The solution is stirred for 15 minutes, followed by the addition of acetic acid (until effervescence stops). The solution is concentrated in vacuo to afford 9.75 g (99%) of the title compound as a brown oil: 1H NMR (400 MHz, CD3OD), 8.686 (d, 1H), 7.828 (d, 1H), 3.937 (s, 3H). LC/MS (M+1)=240.1

WORKUP

后处理

  1. concentrationThe solution is concentrated in vacuo