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
Fourteen grams of 4,5-dihydro-2-(2-phenylethyl)-6H-imidazo[4,5,1-ij]quinolin-6-one obtained in Example 1 was dissolved in dry methanol (140 mL); following the addition of sodium borohydride (0.76 g) under ice cooling and subsequent stirring at room temperature for 1 hr, the solvent was removed under reduced pressure and water was added to the residue, followed by extraction with dichloromethane. The organic layers were combined, washed with water and saturated brine successively, and dried over anhydrous sodium sulfate; thereafter, the solvent was removed under reduced pressure and the residue was purified by silica gel column chromatography (eluting solution: hexane/ethyl acetate) to yield the titled compound as colorless crystals (13.3 g).
WORKUP
后处理
- customthe solvent was removed under reduced pressure and water
- additionwas added to the residue
- extractionfollowed by extraction with dichloromethane
- washwashed with water and saturated brine successively
- dry with materialdried over anhydrous sodium sulfate
- customthereafter, the solvent was removed under reduced pressure
- customthe residue was purified by silica gel column chromatography (eluting solution: hexane/ethyl acetate)