HRID2047268

反应详情

EQUATION

反应方程式

HRID 2047268 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2,6-dichloroisonicotinic acid ethyl ester (14.0 g, 63.6 mmol) in diethylamine (25 mL) is stirred at 100° C. for 7 h. The volatile compounds are evaporated and the residue is purified by CC on silica gel eluting with heptane:EA 9:1 to give 2-chloro-6-diethylamino-isonicotinic acid ethyl ester (10.1 g, contains 2-chloro-6-diethylamino-isonicotinic acid methyl ester which forms during the transfer of the reaction mixture into a round bottom flask using methanol); LC-MS: tR=1.09 min.

WORKUP

后处理

  1. customThe volatile compounds are evaporated
  2. customthe residue is purified by CC on silica gel eluting with heptane:EA 9:1