HRID2181583

反应详情

EQUATION

反应方程式

HRID 2181583 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixture of 3-trifluoromethylbenzyl mercaptan (3.42 g), diisopropylethylamine (2.3 g) and 3-chloro-6-nitro-p-xylene (3.0 g) in dry N-methylpyrrolidinone (20 ml) was heated at 130° C. for 6 hours. On cooling, the mixture was poured into ice-water and the resulting mixture was filtered to give a solid which was washed with ice-water and then air dried. The solid was purified by silica gel chromatography eluting with light petroleum (60-80° C.)/ethyl acetate (9:1) to give the title product as a solid, m.p. 85-7° C.

WORKUP

后处理

  1. temperatureOn cooling
  2. filtrationthe resulting mixture was filtered
  3. customto give a solid which
  4. washwas washed with ice-water
  5. customair dried
  6. customThe solid was purified by silica gel chromatography
  7. washeluting with light petroleum (60-80° C.)/ethyl acetate (9:1)