反应详情

Under a nitrogen stream, 1-(4-methoxybenzyl)-4-methylimidazolidin-2-one (300 mg) described in Preparation Example 52 was dissolved in N,N-dimethylformamide (3 mL), sodium hydride (60 mg) was added under ice-cooling, and the mixture was stirred at room temperature for 30 min. Then, benzoyl chloride (0.17 mL) was added under ice-cooling, and the mixture was stirred at the same temperature for 30 min and at room temperature for 2 hr. To the reaction mixture was added 1N hydrochloric acid, and the mixture was extracted with ethyl acetate. The organic layer was washed with water, 5% aqueous sodium hydrogen carbonate solution and saturated brine, and the solvent was evaporated. The obtained residue was purified by column chromatography (hexane:ethyl acetate) to give the title compound (220 mg).

1. temperaturecooling
2. temperaturecooling
3. stirringthe mixture was stirred at the same temperature for 30 min and at room temperature for 2 hr
4. extractionthe mixture was extracted with ethyl acetate
5. washThe organic layer was washed with water, 5% aqueous sodium hydrogen carbonate solution and saturated brine
6. customthe solvent was evaporated
7. customThe obtained residue was purified by column chromatography (hexane:ethyl acetate)