反应详情

To a solution of 30.1 (162 mg, 0.42 mmol) in 10 mL of EtOAc was added SnCl2.2H2O (469 mg, 2.1 mmol). The mixture was heated to reflux for 3 h. After cooling to room temperature, the mixture was poured into 20 mL of water. Saturated NaHCO3 was added to adjust the pH value of the mixture to 3. The mixture was filtered through Celite to remove solid precipitates. The filtrate was extracted with EtOAc. The EtOAc extract was washed with brine, dried over Na2SO4, and evaporated in vacuo to give 30.2. MS ESI (pos.) m/e calcd for (M+H)+ 361.1. found 361.0.

1. temperatureThe mixture was heated
2. temperatureto reflux for 3 h
3. filtrationThe mixture was filtered through Celite
4. customto remove solid
5. customprecipitates
6. extractionThe filtrate was extracted with EtOAc
7. extractionThe EtOAc extract
8. washwas washed with brine
9. dry with materialdried over Na2SO4
10. customevaporated in vacuo