HRID1588347
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
20 g of 4-hydroxypiperidine was dissolved in 400 ml of dichloromethane, to which 24 g of triethylamine was added. At -60° C., 100 ml of a dichloromethane solution containing 20.7 g of cyclopropanecarbonyl chloride was further added. After completion of the reaction, the reaction solution was extracted with chloroform under salting-out conditions and dried with anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The resultant residue was purified by the use of silica gel column chromatography (elution solvent: dichloroethane), thereby obtaining 32 g of the intended compound (yield 96%).
WORKUP
后处理
- additionwas added
- additionwas further added
- customAfter completion of the reaction
- extractionthe reaction solution was extracted with chloroform under salting-out conditions
- dry with materialdried with anhydrous magnesium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customThe resultant residue was purified by the use of silica gel column chromatography (elution solvent: dichloroethane)