HRID1415653

反应详情

EQUATION

反应方程式

HRID 1415653 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of N-(2-nitrophenyl)-2-chloroacetamide (8.6 g), 2,6-cis-dimethylmorpholine (9.2 g) and ethanol (100 ml) was heated together under reflux for 3 hours. The ethanol was evaporated off and the residue treated with water (100 ml). The resultant suspension was filtered and the solid recrystallised from ethanol to give N-(2-nitrophenyl)-2-(2,6-cis-dimethylmorpholino)acetamide (8.5 g), m.p. 127°-129° C. (with decomposition) which was then dissolved in methanol (100 ml). Platinum oxide (0.3 g) was added to the solution which was then shaken in an atmosphere of hydrogen at atmospheric pressure and laboratory temperature until 1.9 litres of hydrogen had been absorbed. The mixture was filtered and the ethanol evaporated off to give a white solid which was recrystallised from water to give N-(2-aminophenyl)-2-(2,6-cis-dimethylmorpholino)acetamide (5.4 g), m.p. 104°-106° C. (with decomposition).

WORKUP

后处理

  1. temperaturewas heated together
  2. temperatureunder reflux for 3 hours
  3. customThe ethanol was evaporated off
  4. additionthe residue treated with water (100 ml)
  5. filtrationThe resultant suspension was filtered
  6. customthe solid recrystallised from ethanol