HRID1087229

反应详情

EQUATION

反应方程式

HRID 1087229 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-nitro-2',4'-difluorobenzophenone (5.1 g) and methanesulfonyl chloride (14 ml) in pyridine (40 ml) was stirred at room temperature overnight. The mixture was poured into cold 3N hydrochloric acid (200 ml). The insoluble was filtered and dissolved in a mixture of pyridine (20 ml), ethanol (5 ml) and 5% sodium hydroxide (50 ml). The solution was stirred overnight and washed with toluene. The aqueous layer was acidified with hydrochloric acid and the precipitates were filtered to give brown crystals of 2'-(2,4-difluorobenzoyl)-4'-nitromethanesulfonanilide (5.7 g).

WORKUP

后处理

  1. filtrationThe insoluble was filtered
  2. dissolutiondissolved in a mixture of pyridine (20 ml), ethanol (5 ml) and 5% sodium hydroxide (50 ml)
  3. stirringThe solution was stirred overnight
  4. washwashed with toluene
  5. filtrationthe precipitates were filtered