HRID1504009
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
CONDITIONS
反应条件
- 温度
- 180 °C
PROCEDURE
实验过程
A solution of 1,3-diethyl 2-(3-oxocyclohexyl)propanedioate (28.50 g, 111.20 mmol, 1.00 equiv) and sodium chloride (7.02 g, 1.10 equiv) in a mixture of water (4 mL) and DMSO (80 mL) was heated for 24 h at 180° C. in an oil bath. After cooling to r.t, the reaction was diluted with water and extracted with 3×300 mL of ethyl acetate. The organic layers were combined, washed with water and brine, dried over anhydrous sodium sulfate and concentrated under vacuum to give the desired ethyl 2-(3-oxocyclohexyl)acetate (22.7 g, crude) as a yellow oil.
WORKUP
后处理
- temperatureAfter cooling
- extractionextracted with 3×300 mL of ethyl acetate
- washwashed with water and brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under vacuum