反应详情

Diisobutylaluminum hydride (1.0 M in CH2Cl2, 24.8 mmol) was added dropwise to a −78° C. solution of (2) (8.27 mmol, 5.0 g) in CH2Cl2 (40 mL). The mixture was stirred an additional 15 min, quenched with EtOAc (200 mL) and warmed to ambient temperature. Hydrochloric acid (2N, 100 mL) was added slowly and stirred vigorously for 15 min. The layers were separated and the organic layer dried (MgSO4) and concentrated in vacuo. The residue was purified by chromatography (1% acetic acid/acetone) to give 1.54 g (35%) of 4 as a glassy, white solid, m.p. 110-114° C. 1H-NMR and MS (M+1 535) were consistent with the desired product.

1. customquenched with EtOAc (200 mL)
2. additionHydrochloric acid (2N, 100 mL) was added slowly
3. stirringstirred vigorously for 15 min
4. customThe layers were separated
5. dry with materialthe organic layer dried (MgSO4)
6. concentrationconcentrated in vacuo
7. customThe residue was purified by chromatography (1% acetic acid/acetone)