HRID1492275

反应详情

EQUATION

反应方程式

HRID 1492275 的结构方程式

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

A mixture of 4-(2-aminophenyl)morpholine hydrochloride (2.1 g) and N,N-dimethylcyanamide (7 ml) was heated under nitrogen at 165°-170° C. for 12 hours. The reaction mixture was cooled to 10° C. and the precipitate collected by filtration, washed with ether and stirred with 40% aqueous sodium hydroxide solution. The resulting mixture was extracted with dichloromethane and the extract washed with brine and dried. Removal of the solvent yielded a residue which was recrystallised from hexane to give 1,1-dimethyl-2 (2-morpholinophenyl)guanidine (m.p. 144°-145° C.).

WORKUP

后处理

  1. temperaturewas heated under nitrogen at 165°-170° C. for 12 hours
  2. filtrationthe precipitate collected by filtration
  3. washwashed with ether
  4. extractionThe resulting mixture was extracted with dichloromethane
  5. washthe extract washed with brine
  6. customdried
  7. customRemoval of the solvent
  8. customyielded a residue which
  9. customwas recrystallised from hexane