反应详情

A mixture of the product of Step A (3.0 g; 8.61 mmoles) and propargylamine (6.0 ml) in acetonitrile (21 ml) was stirred and heated at reflux temperature under a positive pressure of nitrogen for 18 hours. The reaction mixture was evaporated under reduced pressure and the residue was placed on 70 g of silica gel and chromatographed using a gradient elution of methylene chloride-methanol. The appropriate fractions were combined and evaporated, and the 480 mg of product was recrystallized from isopropanol to yield the title compound containing approximately 2/3 mole of isopropanol, mp 82°-90°. Thin layer chromatography on silica, using methylene chloride:methanol (90:10), gave Rf 0.25.

1. temperatureheated
2. temperatureat reflux temperature under a positive pressure of nitrogen for 18 hours
3. customThe reaction mixture was evaporated under reduced pressure
4. customchromatographed
5. washa gradient elution of methylene chloride-methanol
6. customevaporated
7. customthe 480 mg of product was recrystallized from isopropanol