HRID1461257

反应详情

EQUATION

反应方程式

HRID 1461257 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-amino-5-chlorobenzotrifluoride (14.4 ml, 0.1 mol) and triethylamine (14.0 ml, 0.1 mol) was dissolved in dry tetrahydrofuran, THF (250 ml). To this solution was added with stirring a solution of ethoxalyl chloride in THF (50 ml). After completion of the addition (30 min.) the mixture was stirred at ambient temperature for 3 h, whereafter the precipitated triethylammonium chloride was filtered off, and the filtrate was evaporated in vacuo. This left the crude title compound (24 g) as pale crystals. M.p. 55°-58° C.

WORKUP

后处理

  1. additionTo this solution was added
  2. additionAfter completion of the addition (30 min.) the mixture
  3. filtrationwas filtered off
  4. customthe filtrate was evaporated in vacuo
  5. waitThis left the crude title compound (24 g) as pale crystals