HRID1189629

反应详情

EQUATION

反应方程式

HRID 1189629 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methylamine (13.5 mL, 40% in water) is added to an ice-cooled mixture of 2,4-difluoro-5-nitro-benzoic acid (10.0 g, 49 mmol) in water (100 mL) and it is stirred for 30 min at rt. The mixture is acidified with 6N aq HCl-solution and the precipitate is filtered, washed with water and dried at 60° C. The crude material is recrystallized from MeOH. The final product is slightly contaminated by its regioisomer 4-fluoro-2-methylamino-5-nitro-benzoic acid.

WORKUP

后处理

  1. temperaturecooled
  2. filtrationthe precipitate is filtered
  3. washwashed with water
  4. customdried at 60° C
  5. customThe crude material is recrystallized from MeOH