反应详情

Ethyl 3-bromo-2-oxopropanoate (6.20 mL, 49.40 mmol) was added very carefully to a stirred solution of 2,2-dimethylpropanethioamide (5.79 g, 49.40 mmol) in ethanol (60 mL). The solution was then heated under reflux for 16 h. After cooling, the reaction mixture was diluted with EtOAc, washed with saturated aqueous sodium bicarbonate solution and evaporated in vacuo. Purification by silica gel chromatography (Biotage, 100 g) eluting with EtOAc: iso-hexane, 1:10 gave the sub-title compound as a yellow oil. Yield: 6.56 g

1. temperatureThe solution was then heated
2. temperatureunder reflux for 16 h
3. temperatureAfter cooling
4. washwashed with saturated aqueous sodium bicarbonate solution
5. customevaporated in vacuo
6. customPurification by silica gel chromatography (Biotage, 100 g)
7. washeluting with EtOAc