反应详情

温度

53 °C

A suspension of 1.00 g of (2S,4S)-4-(4-methoxybenzylthio)-2-[(3S)-3-aminopyrrolidin-1-ylcarbonyl]-1-(4-nitrobenzyloxycarbonyl)pyrrolidine hydrochloride [prepared as described in step (ii) above] and 0.47 g of N-(4-nitrobenzyloxycarbonyl)acetamidine in 20 ml of dry acetonitrile was stirred at 53° C. for 2 hours. The reaction mixture was then freed from impurities by filtration, and the filtrate was concentrated by evaporation under reduced pressure. The concentrate was purified by column chromatography through silica gel, using a 45:45:5 by volume mixture of methylene chloride, ethyl acetate and methanol as the eluent, to give 0.89 g of the title compound, as a powder.

1. filtrationThe reaction mixture was then freed from impurities by filtration
2. concentrationthe filtrate was concentrated by evaporation under reduced pressure
3. customThe concentrate was purified by column chromatography through silica gel
4. additionby volume mixture of methylene chloride, ethyl acetate and methanol as the eluent