反应详情

温度

80 °C

A mixture of 1.0 g (2.27 mmol) of (4R)-1-t-butoxycarbonyl-4-(p-toluenesulfonyloxy)-N-t-butyl-L-prolinamide [prepared as described in step (a) above] and 5 g of morpholine was heated at 80° C. for 3 hours, whilst stirring. At the end of this time, the excess morpholine was removed by distillation under reduced pressure, and the residue was mixed with a saturated aqueous solution of sodium hydrogencarbonate. It was then extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate, and the solvent was removed by distillation under reduced pressure. The resulting residue was recrystallized from a mixture of methylene chloride and diethyl ether, to give 650 mg of the title compound as colorless crystals, melting at 172°-173° C.

1. customAt the end of this time, the excess morpholine was removed by distillation under reduced pressure
2. additionthe residue was mixed with a saturated aqueous solution of sodium hydrogencarbonate
3. extractionIt was then extracted with ethyl acetate
4. dry with materialThe extract was dried over anhydrous sodium sulfate
5. customthe solvent was removed by distillation under reduced pressure
6. customThe resulting residue was recrystallized from a mixture of methylene chloride and diethyl ether