反应详情

To a solution of methyl 5-aminopyrazine-2-carboxylate (2 g) in dichloromethane (20 mL) were added pyridine (36.4 mL) and allyl chloroformate (25.2 mL) in 4 divided portions respectively, under ice-cooling, followed by stirring at room temperature overnight. To the reaction mixture was added water under ice-cooling, followed by extraction with ethyl acetate. The organic layer was sequentially washed with 1 M hydrochloric acid, saturated aqueous sodium bicarbonate, and saturated brine. The organic layer was dried over anhydrous magnesium sulfate and concentrated. The obtained solid was collected by filtration while washing with a solvent (hexane:ethyl acetate=3:1) to obtain methyl 5-{[(allyloxy)carbonyl]amino}pyrazine-2-carboxylate (481 mg) as a white solid.

1. temperatureunder ice-cooling
2. temperaturecooling
3. extractionfollowed by extraction with ethyl acetate
4. washThe organic layer was sequentially washed with 1 M hydrochloric acid, saturated aqueous sodium bicarbonate, and saturated brine
5. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
6. concentrationconcentrated
7. filtrationThe obtained solid was collected by filtration
8. washwhile washing with a solvent (hexane:ethyl acetate=3:1)