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 1.73 g (12 mmol) of 2-naphthol in 10 ml of dimethylformamide. The mixture is stirred at room temperature for 3 hours under nitrogen. 200 mg (1.2 mmol) of 4-(2-chloroethyl)-1H-imidazole hydrochloride and tetrabutylammonium iodide (catalytic amount) are added and the mixture is heated at 100° C. for 3 days and then the solvent is evaporated under reduced pressure. The excess 2-naphthol is extracted with diethyl ether under acidic conditions (dilute hydrochloric acid). The aqueous solution is basified with potassium carbonate and the product is extracted with diethyl ether. The ethereal extracts are concentrated and the residue obtained is crystallized from a methanol/water (½) mixture, M.p.: 157°-158° C.
WORKUP
后处理
- temperaturethe mixture is heated at 100° C. for 3 days
- customthe solvent is evaporated under reduced pressure
- extractionThe excess 2-naphthol is extracted with diethyl ether under acidic conditions (dilute hydrochloric acid)
- extractionthe product is extracted with diethyl ether
- concentrationThe ethereal extracts are concentrated
- customthe residue obtained
- customis crystallized from a methanol/water (½) mixture, M.p.: 157°-158° C.