反应详情

To ethyl 2-amino-2-thioxoacetate (4 g, 30 mmol) in ethanol (50 mL) was added pyridine (0.24 g, 3 mmol). 2-Bromo-1-phenylethanone (5 g, 25 mmol) was added after 10 minutes and the mixture was then heated at reflux for 6 hours. The resulting mixture was washed with water and extracted with EtOAc and dried over anhydrous sodium sulfate. The solution was then concentrated under vacuum to give a crude product, which was purified by column chromatography to afford the title compound as a white solid (4.4 g). MS (ESI) m/z 233 (M+H+).

1. temperaturethe mixture was then heated
2. temperatureat reflux for 6 hours
3. washThe resulting mixture was washed with water
4. extractionextracted with EtOAc
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationThe solution was then concentrated under vacuum
7. customto give a crude product, which
8. customwas purified by column chromatography