反应详情

温度

0 °C

In 180 ml of methanol was dissolved 8.39 g (0.0176 mol) of 2S,4S)-N-methanesulfonyl-2 -tert-butyldimethlysilyloxymethyl-4-di-phosphinopyrrolidine [VI], and 11.85 g (0.0348 mol) of 10% hydrogen peroxide was added dropwise to the solution under ice-cooling. The mixture was stirred at 0° C. for one hour and then at room temperature for one hour. To the mixture was then slowly added dropwise a liquid mixture of 8.6 g of 35% hydrochloric acid, 52.7 g of water and 38.7 g of methanol, and the mixture was stirred for 2 hours at room temperature. Any insoluble matter was removed from the mixture by filtration and the filtrate was concentrated under reduced pressure. The concentrate was dissolved in 50 ml of water and the aqueous solution was extracted three times with 100 ml of methylene chloride in each case. The extract was washed with a saturated solution of sodium hydrogen carbonate, dried over magnesium sulfate and concentrated under reduced pressure whereby white crystals were obtained which were then recrystallized from a mixture of ethanol and isopropyl alcohol. Yield 5.3 g (80%), melting point: 138°-139° C.

1. additionwas added dropwise to the solution under ice-
2. temperaturecooling
3. waitat room temperature for one hour
4. additionTo the mixture was then slowly added dropwise
5. stirringthe mixture was stirred for 2 hours at room temperature
6. customAny insoluble matter was removed from the mixture by filtration
7. concentrationthe filtrate was concentrated under reduced pressure
8. dissolutionThe concentrate was dissolved in 50 ml of water
9. extractionthe aqueous solution was extracted three times with 100 ml of methylene chloride in each case
10. washThe extract was washed with a saturated solution of sodium hydrogen carbonate
11. dry with materialdried over magnesium sulfate
12. concentrationconcentrated under reduced pressure whereby white crystals
13. customwere obtained which
14. customwere then recrystallized from a mixture of ethanol and isopropyl alcohol