反应详情

A mixture of the product of Step A (4.0 g, 12.8 mmole) and propargylamine (8.0 ml) in acetonitrile (40 ml) was stirred at reflux temperature under a positive pressure of nitrogen for 16 hours. The reaction mixture was cooled and evaporated to dryness under reduced pressure, and the residue was placed on silica gel and chromatographed by gradient elution using methylene chloride-methanol. Recrystallization from acetonitrile gave the title compound; mp 88°-94° (partial melt at 66°-69°).

1. temperatureat reflux temperature under a positive pressure of nitrogen for 16 hours
2. temperatureThe reaction mixture was cooled
3. customevaporated to dryness under reduced pressure
4. customchromatographed by gradient elution
5. customRecrystallization from acetonitrile