反应详情

To a suspension of (2S ,4S)-4-acetylthio-2-cyano-1-(4-nitrobenzyloxycarbonyl) pyrrolidine (2.60 g) in a mixture of methanol (26 ml) and tetrahydrofuran (52 ml) was added a 28% solution of sodium methoxide in methanol (1.8 ml) at -10°∫-5° C. and the mixture was stirred at the same temperature for 30 minutes. To the mixture was added trityl chloride (2.20 g) at -10°∫-5° C., followed by stirring at the same temperature for 1 hour. The mixture was concentrated under reduced pressure to give a residue. The residue was dissolved in ethyl acetate, washed with water, dried over magnesium sulfate and concentrated under reduced pressure to give a syrup. The syrup was subjected to a column chromatography on silica gel (40 g) and eluted with dichloromethane to give (2S,4S)-2-cyano-1-(4-nitrobenzyloxycarbonyl) -4-tritylthiopyrrolidine (2.45 g).

1. stirringby stirring at the same temperature for 1 hour
2. concentrationThe mixture was concentrated under reduced pressure
3. customto give a residue
4. washwashed with water
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customto give a syrup
8. washeluted with dichloromethane