HRID1486583

反应详情

EQUATION

反应方程式

HRID 1486583 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 4-amino-2,6-dichlorobenzonitrile (500 mg, 2.67 mmol, Eq: 1.00), thiophosgene (1.35 g, 900 μl, 11.7 mmol, Eq: 4.39), triethylamine (875 mg, 1.2 ml, 8.64 mmol, Eq: 3.23) in benzene (30 ml) was heated at reflux overnight. The brown reaction mixture was concentrated and chromatographed (80 g Analogix, 0 to 5% ethyl acetate/hexane) to give 436 mg (71%) of desired product as a light brown solid.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux overnight
  3. concentrationThe brown reaction mixture was concentrated
  4. customchromatographed (80 g Analogix, 0 to 5% ethyl acetate/hexane)