反应详情

温度

85 °C

To a suspension of 92 (3.3 g, 6.8 mmol) in EtOH (8 ml) was added concentrated HCl (7 ml) and distilled water (4 ml). The mixture was heated at 80-90° C. for 2.5 h, cooled to room temperature and concentrated under reduced pressure. The remaining residue was subjected to azeotropic distillation with EtOH followed by neutralization with saturated aqueous NaHCO3. The solid that precipitated was filtered and washed with water, and the filtrate was extracted with EtOAc. The solid and EtOAc extract were combined, evaporated under reduced pressure and the residue was collected and dried to afford the title compound 93 (2.4 g, 100% yield) as a yellow solid. MS (m/z) 357.0 (M+H).

1. distillationdistilled water (4 ml)
2. temperaturecooled to room temperature
3. concentrationconcentrated under reduced pressure
4. distillationThe remaining residue was subjected to azeotropic distillation with EtOH
5. customThe solid that precipitated
6. filtrationwas filtered
7. washwashed with water
8. extractionthe filtrate was extracted with EtOAc
9. extractionThe solid and EtOAc extract
10. customevaporated under reduced pressure
11. customthe residue was collected
12. customdried