HRID132716
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
To 0.03 mol 1,4-dihydroxymethylcyclohexane were added 30 ml tetrahydrofuran and 0.09 mol pyridine, then added 0.075 mol benzoyl chloride with stirring. The reaction was heated refluxing for 4 hours, cooled and added 20 ml saturated saline. The reaction mixture was extracted with ethyl acetate, and the extract was dried over anhydrous sodium sulfate, filtered. After removing solvent, the crude was purified by recrystallization from ethyl acetate and petroleum ether (2:1 v/v) to give 1,4-di(benzoyloxymethyl)cyclohexane as a white solid. The yield was 95%, and m.p. was 111-113° C.
WORKUP
后处理
- temperatureThe reaction was heated
- temperaturerefluxing for 4 hours
- temperaturecooled
- additionadded 20 ml saturated saline
- extractionThe reaction mixture was extracted with ethyl acetate
- dry with materialthe extract was dried over anhydrous sodium sulfate
- filtrationfiltered
- customAfter removing solvent
- customthe crude was purified by recrystallization from ethyl acetate and petroleum ether (2:1 v/v)