HRID1058347

反应详情

EQUATION

反应方程式

HRID 1058347 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturecooled in a water bath
  2. washthe reaction mixture was washed with water (2×20 mL)
  3. extractionEach of the aqueous layers was extracted with dichloromethane
  4. dry with materialthe combined organic layers were dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated