反应详情

Compound 96B (5.5 g, 10.14 mmol) in THF (100 mL) and methanol (20 mL) was treated NaBH4 (0.767 g, 20.28 mmol). The reaction mixture was heated under reflux for 1 hour. The solvents were removed under vacuum. The residue was re-dissolved in EtOAc and treated with water. The organic layer was separated, and the aqueous layer was extracted with additional EtOAc. The combined organic layers were washed with brine, dried (MgSO4), filtered, and concentrated. The residue was purified by flash chromatography to give 5.13 g of the title compound 96C (93%): APCI (+)LC/MS: 545 (M+H)+.

1. temperatureThe reaction mixture was heated
2. temperatureunder reflux for 1 hour
3. customThe solvents were removed under vacuum
4. dissolutionThe residue was re-dissolved in EtOAc
5. additiontreated with water
6. customThe organic layer was separated
7. extractionthe aqueous layer was extracted with additional EtOAc
8. washThe combined organic layers were washed with brine
9. dry with materialdried (MgSO4)
10. filtrationfiltered
11. concentrationconcentrated
12. customThe residue was purified by flash chromatography