反应详情

To a solution of 73A (3.06 g, 11.9 mmol) in 50 mL CH2Cl2 at −78° C., was added a solution of diisobutylaluminum hydride (35.7 mL, 35.7 mmol, 1M in hexanes). The mixture was removed from the cooling bath, stirred 1 h, then recooled to −50° C. and quenched with EtOAc (2 mL). The reaction mixture was diluted with H2O, then extracted with EtOAc (3×). The combined organic extract washed with brine, dried (Na2SO4), filtered through a 1″ pad of SiO2, then concentrated to afford 2.34 g of 73B as a colorless oil. MS (ESI) m/z 197.1 (M-OH)+.

1. customThe mixture was removed from the cooling bath
2. customrecooled to −50° C.
3. customquenched with EtOAc (2 mL)
4. additionThe reaction mixture was diluted with H2O
5. extractionextracted with EtOAc (3×)
6. extractionThe combined organic extract
7. washwashed with brine
8. dry with materialdried (Na2SO4)
9. filtrationfiltered through a 1″ pad of SiO2
10. concentrationconcentrated