反应详情

A solution of alcohol (5) (0.29 g, 1 mmol) in dichloromethane (10 ml) was treated with thionyl chloride (1 g) and stirred at room temperature under nitrogen overnight. The solvent was removed on a rotary evaporator (bath temperature below 28° C.). Dichloromethane (10 ml) was added and stripped under the same conditions twice. The solid residue was taken in water (8 ml) and washed with MTBE (2×15 ml). The resulting aqueous solution contains pure (6) (LCMS) and was used as such in the next step.

1. customThe solvent was removed on a rotary evaporator (bath temperature below 28° C.)
2. additionDichloromethane (10 ml) was added
3. washwashed with MTBE (2×15 ml)