HRID2308585

反应详情

EQUATION

反应方程式

HRID 2308585 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A suspension of 5-[2'-chloro-4'-(trifluoromethyl)phenoxy]-2-nitrobenzamide (54.1 g; 0.15 mol) and 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulphide (LAWESSON's reagent) (28 g; 0.075 mol) in toluene (250 cc) is prepared. It is heated to 100° C., with stirring, and the heating is continued for 1 hour at this temperature. The toluene is removed by evaporation and the residue is purified by chromatography. This gives a yellow solid of 5-[2'-chloro-4'-(trifluoromethyl)phenoxy]-2-nitrothiobenzamide (36.4 g; yield 65%) melting at 152° C. and having the formula: ##STR21##

WORKUP

后处理

  1. customis prepared
  2. customThe toluene is removed by evaporation
  3. customthe residue is purified by chromatography