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
240 mg (60% in oil, 6 mmol) of sodium hydride are added to a solution of 2.34 g (12 mmol) of 4-hydroxybenzophenone in 10 ml of dimethylformamide. The mixture is stirred at room temperature for 1 hour under nitrogen. 200 mg (1.2 mmol) of 4-(2-chloroethyl)-1H-imidazole hydrochloride and tetrabutylammonium iodide (catalytic amount) are then added. The mixture is heated at 100° C. for 2 days and the solvent is then evaporated under reduced pressure. Dilute hydrochloric acid is added to the oily residue and the excess hydroxybenzophenone is extracted with diethyl ether. The aqueous solution is basified with potassium carbonate and the product is extracted with diethyl ether. The title compound is converted to the dioxalate. Crystallization from an ethanol/diethyl ether (2/1) mixture gives a pure product, M.p.: 193°-194° C.
WORKUP
后处理
- temperatureThe mixture is heated at 100° C. for 2 days
- customthe solvent is then evaporated under reduced pressure
- additionDilute hydrochloric acid is added to the oily residue
- extractionthe excess hydroxybenzophenone is extracted with diethyl ether
- extractionthe product is extracted with diethyl ether
- customCrystallization from an ethanol/diethyl ether (2/1) mixture
- customgives a pure product, M.p.: 193°-194° C.