反应详情

To a stirred solution of chloromethyl chloroformate (7.09 g, 5.5 mmol) in heptane (100 mL) at −20° C. add a solution of diethylamine (10.4 g, 14.7 mmol) in heptane (50 mL), dropwise. Maintain the internal temperature between −15° C. to −5° C. and after 1 h quench the reaction with water. Separate the layers and wash the organic phase with 10% aqueous HCl, water and NaHCO3 solution. Dry the organic layer (MgSO4), filter and concentrate under reduced pressure to obtain 8.3 g of the title compound.

1. temperatureMaintain the internal temperature between −15° C. to −5° C.
2. customafter 1 h quench
3. customthe reaction with water
4. customSeparate the layers
5. washwash the organic phase with 10% aqueous HCl, water and NaHCO3 solution
6. dry with materialDry the organic layer (MgSO4)
7. filtrationfilter
8. concentrationconcentrate under reduced pressure