反应详情

2.24 g (0.02 mole) of potassium t-butoxide were added to a solution of 3.55 g (0.01 mole) of 1-t-butoxycarbonyl-3-(p-toluenesulfonyloxymethyl)pyrrolidine [prepared as described in Step (3) above] dissolved in 50 ml of tetrahydrofuran. The mixture was then stirred at room temperature for 3 hours, after which it was poured into water and then extracted with ethyl acetate. The ethyl acetate extract was washed with water, dried and concentrated by evaporation under reduced pressure. The residue was subjected to column chromatography through silica gel eluted with a 5:95 by volume mixture of ethyl acetate and toluene, to give 0.79 g of 1-t-butoxycarbonyl-3-methylenepyrrolidine as a pale yellow liquid.

1. extractionextracted with ethyl acetate
2. extractionThe ethyl acetate extract
3. washwas washed with water
4. customdried
5. concentrationconcentrated by evaporation under reduced pressure
6. washeluted with a 5:95 by volume mixture of ethyl acetate and toluene