反应详情

To a suspension of 3-dimethylamino-1-(4-methylpyridin-2-yl)prop-2-en-1-one (0.78 g) and cyanoguanidine (1.38 g) in ethanol (8 ml) was added a solution of sodium methoxide in methanol (28%, 1.49 ml), and the mixture was refluxed for 2 hours. The mixture was neutralized with 1N hydrochloric acid and extracted with ethyl acetate and tetrahydrofuran (3:1). The organic layer was washed with brine, dried over sodium sulfate and evaporated under reduced pressure. The residue was purified by column chromatography (silica gel 75 g, 10% methanol in dichloromethane). The solid obtained was triturated with 2-propanol, filtered and dried to give N-(4-(4-methylpyridin-2-yl)-pyrimidin-2-yl)cyanamide (325 mg).

1. temperaturethe mixture was refluxed for 2 hours
2. extractionextracted with ethyl acetate and tetrahydrofuran (3:1)
3. washThe organic layer was washed with brine
4. dry with materialdried over sodium sulfate
5. customevaporated under reduced pressure
6. customThe residue was purified by column chromatography (silica gel 75 g, 10% methanol in dichloromethane)
7. customThe solid obtained
8. customwas triturated with 2-propanol
9. filtrationfiltered
10. customdried