HRID1588683

反应详情

EQUATION

反应方程式

HRID 1588683 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-(2-morpholinophenyl)thiourea (10.5 g) was suspended in boiling water (80 ml) and a solution of potassium hydroxide (25.2 g) in hot water (70 ml) was added. The mixture was heated to 90°0 C. and aliquot portions of a hot solution of lead acetate trihydrate (17.5 g) in water (80 ml) added and the mixture heated under reflux for 10 minutes and cooled to ambient temperature. The mixture was filtered and the filtrate acidified with acetic acid to pH 6. The solid which formed was separated by filtration, washed with water and recrystallised from ethylacetate to give N-(2-morpholinophenyl)cyanamide (m.p. 175°-176° C.).

WORKUP

后处理

  1. temperatureThe mixture was heated to 90°0 C
  2. temperaturethe mixture heated
  3. temperatureunder reflux for 10 minutes
  4. filtrationThe mixture was filtered
  5. customThe solid which formed
  6. customwas separated by filtration
  7. washwashed with water
  8. customrecrystallised from ethylacetate