HRID132708
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
To 5.5 g pyrocatechol were added 50 ml tetrahydrofuran and 12.1 ml pyridine with stirring. Then to the resulting homogeneous mixture was slowly added 14.5 ml benzoyl chloride, and the reaction was stirred at room temperature for 1 hour, then heated refluxing for 4 hours. Next, 70 ml water was added to dissolve the resulting salt. The reaction mixture was extracted with toluene. Organic phase was separated, washed with saturated saline for two times, dried over anhydrous sodium sulfate. Removing solvent gave a white solid. After recrystallizing from ethyl acetate, 1,2-phenylene dibenzoate was obtained as a white crystal, the yield was 94%, and m.p. was 75-77° C.
WORKUP
后处理
- stirringthe reaction was stirred at room temperature for 1 hour
- temperatureheated
- temperaturerefluxing for 4 hours
- dissolutionto dissolve the resulting salt
- extractionThe reaction mixture was extracted with toluene
- customOrganic phase was separated
- washwashed with saturated saline for two times
- dry with materialdried over anhydrous sodium sulfate
- customRemoving solvent gave a white solid
- customAfter recrystallizing from ethyl acetate