反应详情

Subsequently, to a suspension of 60% sodium hydride (8.41 g, 210 mmol) in tetrahydrofuran (120 mL) is added dropwise a solution of the above lactic morpholinamide (32.1 g) in tetrahydrofuran (150 mL) under nitrogen atmosphere with stirring under ice-cooling, and the mixture is heated with stirring at 50° C. for 30 minutes. After cooling with ice, to the mixture is added dropwise a solution of p-toluene-sulfonyl chloride (45.8 g, 234 mmol) in tetrahydrofuran (180 mL), and the mixture is stirred at room temperature for 4 hours. To the mixture is added 1N aqueous hydrochloric acid solution, and the mixture is extracted with ethyl acetate. The organic layer is washed with water and a saturated brine, dried over anhydrous magnesium sulfate, and the solvent is evaporated under reduced pressure. To the resulting oily residue is added diethyl ether, and the precipitated crystals are collected by filtration, washed with diethyl ether, and dried under reduced pressure to give the title compound (36.1 g, yield: 58%).

1. temperaturecooling
2. temperaturethe mixture is heated
3. stirringwith stirring at 50° C. for 30 minutes
4. temperatureAfter cooling with ice, to the mixture
5. stirringthe mixture is stirred at room temperature for 4 hours
6. extractionthe mixture is extracted with ethyl acetate
7. washThe organic layer is washed with water
8. dry with materiala saturated brine, dried over anhydrous magnesium sulfate
9. customthe solvent is evaporated under reduced pressure
10. additionTo the resulting oily residue is added diethyl ether
11. filtrationthe precipitated crystals are collected by filtration
12. washwashed with diethyl ether
13. customdried under reduced pressure