反应详情

To 360 ml of tetrahydrofuran was added 3.98 g (0.105 mol) of lithium aluminum hydride, and the mixture was stirred. To this mixture was slowly added dropwise a solution of 16.6 g (0.07 mol) of (2S,4R)-N-methanesulfonyl-4-hydroxyproline ethyl ester [III] in 200 ml of tetrahydrofuran under agitation and ice-cooling. After stirring the suspension at 0° C. for 3 hours and then at room temperature for 3 hours, 14 ml of water was added dropwise in small portions to the suspension under ice-cooling, and thereafter the mixture was stirred for 30 minutes. Any insoluble matter was removed by filtration and the filtrate was concentrated until dryness under reduced pressure whereby 11.9 g (yield: 87%) of an oily substance was obtained.

1. temperaturecooling
2. stirringAfter stirring the suspension at 0° C. for 3 hours
3. temperaturecooling
4. stirringthe mixture was stirred for 30 minutes
5. customAny insoluble matter was removed by filtration
6. concentrationthe filtrate was concentrated until dryness under reduced pressure whereby 11.9 g (yield: 87%) of an oily substance
7. customwas obtained