HRID237074

反应详情

EQUATION

反应方程式

HRID 237074 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4.4 g (0.02 mole) of N-benzyl-N-chloromethylcarbamoyl chloride and 2.0 g (0.02 mole) of 1,3-dimethylthiourea was dissolved in 50 ml of ethyl alcohol and heated under reflux with stirring for 2 hours. After addition of 20 ml of a saturated aqueous potassium carbonate solution, the mixture was extracted with 100 ml of benzene. The benzene layer was washed with water, dried, and freed from the benzene by distillation under reduced pressure to obtain 4.0 g of crude crystals which were recrystallized from ether. Yield 3.2 g (63%); m.p. 93°-95° C.

WORKUP

后处理

  1. temperatureheated
  2. temperatureunder reflux
  3. extractionthe mixture was extracted with 100 ml of benzene
  4. washThe benzene layer was washed with water
  5. customdried
  6. distillationfreed from the benzene by distillation under reduced pressure