反应详情

Under a nitrogen stream, sodium borohydride (0.65 g) was suspended in tetrahydrofuran (25 mL), boron trifluoride diethyl ether complex (2.63 mL) was added dropwise under ice-cooling, and the mixture was stirred at the same temperature for 15 min. Then, a solution of 3-(4-methoxybenzyl)-5-methylimidazolidine-2,4-dione (2.00 g) described in Preparation Example 51 in tetrahydrofuran (25 ml) was added under ice-cooling, and the mixture was stirred at the same temperature for 30 min and at room temperature overnight. To the reaction mixture were added dropwise methanol and 0.5N hydrochloric acid, and the mixture was stirred at room temperature for 1 hr. The solvent was evaporated from the reaction mixture, water was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, water and saturated brine, and the solvent was evaporated. The obtained residue was purified by column chromatography (hexane:ethyl acetate) to give the title compound (1.16 g).

1. additionboron trifluoride diethyl ether complex (2.63 mL) was added dropwise under ice-
2. temperaturecooling
3. additionwas added under ice-
4. temperaturecooling
5. stirringthe mixture was stirred at the same temperature for 30 min and at room temperature overnight
6. stirringthe mixture was stirred at room temperature for 1 hr
7. customThe solvent was evaporated from the reaction mixture, water
8. additionwas added
9. extractionthe mixture was extracted with ethyl acetate
10. washThe organic layer was washed with 1N hydrochloric acid, water and saturated brine
11. customthe solvent was evaporated
12. customThe obtained residue was purified by column chromatography (hexane:ethyl acetate)