反应详情

温度

50 °C

The product of Step (d) (0.5 g, 2.2 mmol) was dissolved in acetonitrile (1 ml). In a separate flask, diketene (0.17 ml, 2.2 mmol, stabilized with copper sulfate) was dissolved in acetonitrile (1 ml). The diketene solution was added to the amine suspension In three portions, the reaction mixture was sealed and heated to 50° C. for 18 hours. The solvent was evaporated to dryness and purified by silica gel chromatography (5% MeOH/CH2Cl2) to afford the title compound, (0.3 g, 44%); MS (ES+) m/e 313 [M+H]+.

1. customthe reaction mixture was sealed
2. customThe solvent was evaporated to dryness
3. custompurified by silica gel chromatography (5% MeOH/CH2Cl2)