反应详情

A 100-mL round bottom flask was charged with ethyl 2-ethyl-3-oxo-butanoate (5 g, 90% purity, 28 mmol), ammonium acetate (22 g, 280 mmol, 10 eq.), ammonia (2N in EtOH, 14 ml, 1 eq.), anhydrous sodium sulfate (8 g, 56 mmol, 2 eq.) and MeOH (30 ml). The resulting mixture was stirred at room temperature overnight. The volatile material was removed under reduced pressure and the residue was treated with dichloromethane (40 ml). Insoluble material was removed by filtration and washed with dichloromethane (2×20 ml). The organics was washed with aqueous sodium bicarbonate, dried over Na2SO4. Removal of solvent gave ethyl (Z)-3-amino-2-ethyl-but-2-enoate (4.1 g, 82% yield) as a white solid.

1. customThe volatile material was removed under reduced pressure
2. additionthe residue was treated with dichloromethane (40 ml)
3. customInsoluble material was removed by filtration
4. washwashed with dichloromethane (2×20 ml)
5. washThe organics was washed with aqueous sodium bicarbonate
6. dry with materialdried over Na2SO4
7. customRemoval of solvent