HRID1957260
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
50 ml of trimethyl orthoformate were added to 40.0 g of montmorillonite K-10 in 250 ml of anhydrous dichloromethane, after which a solution of 20.0 g of 3-chloro-2-(4-chloro-3-formylphenyl)-5-trifluoromethylpyridine in 50 ml of dichloromethane was added dropwise while stirring and cooling in ice. After stirring at 23° C. for 20 hours, the clay was removed and thoroughly washed with dichloromethane. The dichloromethane phase was concentrated. The residue was purified by chromatography on silica gel with cyclohexane/ethyl acetate (10:1). Yield: 22.1 g (96%) of a colorless oil.
WORKUP
后处理
- temperaturecooling in ice
- stirringAfter stirring at 23° C. for 20 hours
- customthe clay was removed
- washthoroughly washed with dichloromethane
- concentrationThe dichloromethane phase was concentrated
- customThe residue was purified by chromatography on silica gel with cyclohexane/ethyl acetate (10:1)