HRID1058347
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
A 1M solution of sulfuryl chloride in dichloromethane (25 mL, 25 mmol) was added to a solution of 4-methyl-3-oxopentanoic acid ethyl ester (3.95 g, 25 mmol) in dichloromethane (15 mL) cooled in a water bath. The solution was stirred at room temperature for 2 h and then the reaction mixture was washed with water (2×20 mL). Each of the aqueous layers was extracted with dichloromethane and the combined organic layers were dried (MgSO4), filtered and evaporated to give 2-chloro-4-methyl-3-oxopentanoic acid ethyl ester (5.0 g, 104% of the theoretical amount). This was used directly in the next step without purification.
WORKUP
后处理
- temperaturecooled in a water bath
- washthe reaction mixture was washed with water (2×20 mL)
- extractionEach of the aqueous layers was extracted with dichloromethane
- dry with materialthe combined organic layers were dried (MgSO4)
- filtrationfiltered
- customevaporated