HRID1492275
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperaturewas heated under nitrogen at 165°-170° C. for 12 hours
- filtrationthe precipitate collected by filtration
- washwashed with ether
- extractionThe resulting mixture was extracted with dichloromethane
- washthe extract washed with brine
- customdried
- customRemoval of the solvent
- customyielded a residue which
- customwas recrystallised from hexane