反应详情

Compound 94E (0.91 g, 1.351 mmol) in THF (30 mL) and methanol (5 mL) was treated with NaBH4 (0.102 g, 2.7 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 0.75 g of the title compound 94F (82%): APCI (+)LC/MS: 675 (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