HRID2081897

反应详情

EQUATION

反应方程式

HRID 2081897 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

0.246 mol (79 g) of 2-amino-3-nitro-5-methyl-N-tosylaniline is dissolved in 260 ml of normal sodium hydroxide solution at 40° C. 0.286 mol (30 ml) of methyl sulphate is added gradually in the course of 3 hours, the temperature being kept at about 40° C. Towards the end of the addition of the methyl sulphate, the pH of the reaction medium is kept alkaline by simultaneously adding 20 ml of normal sodium hydroxide solution. After cooling to about 10° C., the expected product which has precipitated is filtered off. It is washed with a normal sodium hydroxide solution and then with water and recrystallised from acetic acid. After drying in vacuo, it melts at 208° C.

WORKUP

后处理

  1. custombeing kept at about 40° C
  2. customthe expected product which has precipitated
  3. filtrationis filtered off
  4. washIt is washed with a normal sodium hydroxide solution
  5. customwith water and recrystallised from acetic acid
  6. customAfter drying in vacuo, it melts at 208° C.