反应详情

温度

0 °C

A 100 mL round bottom flask was charged with 83.18D (0.92 g, 2.2 mmol), DCM (22 mL), and diiodomethane (available from Aldrich) (0.27 mL, 3.3 mmol) and cooled to 0° C. under N2. To the cold solution was added diethylzinc (1.0 M in heptane) (available from Aldrich) (3.3 mL, 3.3 mmol) at a rapid drip. The colorless mixture was stirred for 5 minutes. The cooling bath was removed, and the mixture was stirred for 2 hours at ambient temperature. The reaction was quenched with saturated aqueous NH4Cl and diluted with EtOAc. The organic phase was washed with 1 M Na2S2O3 and brine, dried (MgSO4), and concentrated. The residue was purified by silica gel flash chromatography (0-15% EtOAc/hexane) to afford 83.18E (0.81 g, 85%) as a colorless oil.

1. customThe cooling bath was removed
2. stirringthe mixture was stirred for 2 hours at ambient temperature
3. customThe reaction was quenched with saturated aqueous NH4Cl
4. additiondiluted with EtOAc
5. washThe organic phase was washed with 1 M Na2S2O3 and brine
6. dry with materialdried (MgSO4)
7. concentrationconcentrated
8. customThe residue was purified by silica gel flash chromatography (0-15% EtOAc/hexane)