反应详情

A mixture of the product of Step A (4.3 g, 14.7 mmole) and propargylamine (8.6 ml) in acetonitrile (43 ml) was stirred at reflux temperature under a positive pressure of nitrogen for 15 hours then at room temperature for an additional 48 hours. The reaction mixture was filtered to remove by-product and the filtrate was evaporated under reduced pressure. The residual gum was placed on silica gel and chromatographed by gradient elution using methylene chloride-methanol. The appropriate fractions were combined and the product recrystallized from acetonitrile to give the title compound; mp 112.5°-115°.

1. temperatureat reflux temperature under a positive pressure of nitrogen for 15 hours
2. filtrationThe reaction mixture was filtered
3. customto remove by-product
4. customthe filtrate was evaporated under reduced pressure
5. customchromatographed by gradient elution
6. customthe product recrystallized from acetonitrile