反应详情

温度

0 °C

A 250 mL round bottom flask was charged with 66.56D (mixture of diastereomers) (0.61 g, 1.7 mmol), DCM (10 mL), and TEA (0.28 mL, 2.0 mmol) and cooled to 0° C. To the cold solution was added methanesulfonyl chloride (available from Aldrich) (0.16 mL, 2.0 mmol) dropwise. The cooling bath was removed, and the mixture was stirred for 1 hour at ambient temperature. The mixture was diluted with EtOAc, washed with water and brine, dried (MgSO4), and concentrated. The crude product was purified by silica gel flash chromatography (0-40% EtOAc/hexane) to afford 66.56E (mixture of diastereomers) (0.69 g, 93% yield) as a colorless oil.

1. customThe cooling bath was removed
2. additionThe mixture was diluted with EtOAc
3. washwashed with water and brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated
6. customThe crude product was purified by silica gel flash chromatography (0-40% EtOAc/hexane)