反应详情

A solution of 3.0 g of cyclohexanol and 2.4 ml of pyridine in 30 ml of methylene chloride is cooled to -78° C. and, with stirring, 2.4 ml of chloromethyl chloroformate is added dropwise to the solution. After completion of addition, a cold bath is removed. The mixture is stirred at room temperature for 16 hours, washed with three 30-ml portions of saturated aqueous sodium chloride and dried over anhydrous magnesium sulfate. The solvent is then distilled off under reduced pressure to give 4.5 g of colorless oil, which is crystallized from ligroine giving the title compound as colorless crystals melting at 36°-37° C.

1. additionAfter completion of addition, a cold bath
2. customis removed
3. stirringThe mixture is stirred at room temperature for 16 hours
4. washwashed with three 30-ml portions of saturated aqueous sodium chloride
5. dry with materialdried over anhydrous magnesium sulfate
6. distillationThe solvent is then distilled off under reduced pressure