反应详情

NaBH4 (1.06 g, 28 mmol, 3.0 equiv) was added to a solution of 2.21.1a (3.5 g, 9.4 mmol, 1.0 equiv) in THF (10.0 mL) and MeOH (30 mL) at 0° C. The resulting mixture was stirred at room temperature for 1 hour, after which, another 0.3 g of NaBH4 (300 mg, 7.8 mmol, 0.8 equiv) was added. After stirring at room temperature for 30 minutes, the solvent was removed under vacuum. The residue was dissolved in EtOAc and saturated aqueous NaHCO3 solution was added. The phases were separated and the organic layer was washed with brine, dried over Na2SO4 and concentrated. The crude material was used in the next step with no further purification. MS m/z (M+Na): 354

1. stirringAfter stirring at room temperature for 30 minutes
2. customthe solvent was removed under vacuum
3. dissolutionThe residue was dissolved in EtOAc
4. additionsaturated aqueous NaHCO3 solution was added
5. customThe phases were separated
6. washthe organic layer was washed with brine
7. dry with materialdried over Na2SO4
8. concentrationconcentrated
9. customThe crude material was used in the next step with no further purification