反应详情

温度

-20 °C

A solution of diisobutylaluminum hydride (12.0 ml, 12.0 mmol, 1M in THF) was added dropwise to a solution of the product from STEP 2 (1.5 g, 6.0 mmol) in 15 ml THF at −20° C. The resulting mixture was stirred at −20° C. for 20 min and allowed to warm to room temperature. After 3 h, the reaction was diluted with ether (70 ml) and washed with 50 ml of aqueous 1M tartaric acid. The organic extracts were dried with MgSO4, filtered and concentrated. The residue was purified by chromatography (SiO2, ethyl acetate/hexane=1/3) to afford 0.58 g of a viscous. The 1H NMR spectrum of the product was consistent for the proposed structure.

1. temperatureto warm to room temperature
2. waitAfter 3 h
3. washwashed with 50 ml of aqueous 1M tartaric acid
4. dry with materialThe organic extracts were dried with MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by chromatography (SiO2, ethyl acetate/hexane=1/3)
8. customto afford 0.58 g of a viscous