反应详情

A mixture of 1,1-dimethyl-3-(2-morpholinophenyl)thiourea (2.65 g prepared as described in Example 232), lead acetate trihydrate (3.8 g), saturated ethanolic ammonia solution (25 ml), potassium hydroxide (1.12 g) and ethanol (20 ml) where heated at 90°-95° C. is a sealed stainless steel pressure vessel for 5 hours. The reaction mixture was filtered and the solid collected washed with ethanol. The washings were added to the filtrate and the volume reduced by evaporation. Ice was added and the resulting solid was collected by filtration, washed with water and dried to give 1,1-dimethyl-2-(2-morpholinophenyl)guanidine (m.p. 141°-142° C.) which was recrystallised from hexane.

1. temperatureheated at 90°-95° C.
2. customfor 5 hours
3. filtrationThe reaction mixture was filtered
4. customthe solid collected
5. washwashed with ethanol
6. additionThe washings were added to the filtrate
7. customthe volume reduced by evaporation
8. additionIce was added
9. filtrationthe resulting solid was collected by filtration
10. washwashed with water
11. customdried