反应详情

A mixture of 4-(2-aminophenyl)morpholine hydrochloride (6.5 g) and valeronitrile (35 ml) were heated at 160°-165° C. under nitrogen for 25 hours and then cooled. The mixture was treated with aqueous sodium hydroxide and the basified mixture was extracted with dichloromethane. The solvent was removed by evaporation and the residue distilled under a pressure of 50 mm Hg to remove half the unreacted valeronitrile. A solid separated on cooling which was separated by filtration, washed with hexane (50 ml) and recrystallised from hexane to give N-(2-morpholinophenyl)valeramidine. (m.p. 135°-136° C.).

1. temperaturewere heated at 160°-165° C. under nitrogen for 25 hours
2. temperaturecooled
3. extractionthe basified mixture was extracted with dichloromethane
4. customThe solvent was removed by evaporation
5. distillationthe residue distilled under a pressure of 50 mm Hg
6. customto remove half the unreacted valeronitrile
7. customA solid separated
8. temperatureon cooling which
9. customwas separated by filtration
10. washwashed with hexane (50 ml)
11. customrecrystallised from hexane