HRID2081894

反应详情

EQUATION

反应方程式

HRID 2081894 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.087 mol (28 g) of 2-amino-3-nitro-5-methyl-N-tosylaniline is dissolved in 85 ml of DMF heated beforehand on a boiling water-bath. 9.7 g of quicklime are then added and 0.174 mol (21.75 g) of glycol bromohydrin is then introduced gradually, in the course of 30 minutes and whilst stirring, the heating on the boiling water-bath being maintained. After 11/2 hours, the reaction medium is filtered hot and the filtrate is then poured into 250 ml of iced water. The expected product precipitates. It is filtered off, washed with water and dried in vacuo. After recrystallisation from acetic acid and drying in vacuo, it melts at 201° C.

WORKUP

后处理

  1. filtrationAfter 11/2 hours, the reaction medium is filtered hot
  2. additionthe filtrate is then poured into 250 ml of iced water
  3. customThe expected product precipitates
  4. filtrationIt is filtered off
  5. washwashed with water
  6. customdried in vacuo
  7. customAfter recrystallisation from acetic acid
  8. customdrying in vacuo, it melts at 201° C.