反应详情

A mixture of 1,1-dimethyl-3-(2-morpholinophenyl)thiourea (2.65 g prepared as described in Example 232), n-propylamine (1.6 ml), lead acetate trihydrate (3.8 g), potassium hydroxide (1.2 g) and ethanol (25 ml) was heated under reflux for 4 hours. A further amount of n-propylamine (1.6 ml) was added and the mixture heated under reflux for a further 8 hours. The reaction mixture yielded a residue which was extracted with ether. The extract was decolourised with charcoal, filtered and the solvent removed to leave a sticky solid which was dissolved in methanol (10 ml) and treated with fumaric acid to give 1,3-di-(n-propyl)-2-(2-morpholinophenyl)guanidine hemifumarate (m.p. 212°-214° C.) which was recrystallised from a 1:2 mixture of methanol and ether.

1. temperaturewas heated
2. temperatureunder reflux for 4 hours
3. temperaturethe mixture heated
4. temperatureunder reflux for a further 8 hours
5. customThe reaction mixture yielded a residue which
6. extractionwas extracted with ether
7. filtrationfiltered
8. customthe solvent removed
9. customto leave a sticky solid which