反应详情

A mixture of N-(phenoxycarbonylamino)-1,2,3,6-tetrahydropyridine (2.61 g), 4-aminopyrimidine (0.95 g) and 4-dimethylaminopyridine (1.83 g) in 1,2-dichloroethane (80 ml) was refluxed for 2.5 hours. The reaction mixture was evaporated to dryness. The crude residue was dissolved in ethyl acetate (50 ml) and washed with water (50 ml), and then extracted with 5% hydrochloric acid (30 ml×2). The extract was neutralized with sodium bicarbonate and further extracted with chloroform (30 ml×2). The chloroform layer was washed with water (50 ml), dried over magnesium sulfate and evaporated to give N-[(4-pyrimidinylcarbamoyl)amino]-1,2,3,6-tetrahydropyridine (1.41 g), which was recrystallized from ethyl acetate.

1. temperaturewas refluxed for 2.5 hours
2. customThe reaction mixture was evaporated to dryness
3. dissolutionThe crude residue was dissolved in ethyl acetate (50 ml)
4. washwashed with water (50 ml)
5. extractionextracted with 5% hydrochloric acid (30 ml×2)
6. extractionfurther extracted with chloroform (30 ml×2)
7. washThe chloroform layer was washed with water (50 ml)
8. dry with materialdried over magnesium sulfate
9. customevaporated