反应详情

Trifluoroacetic acid (0.50 mL) was a add to a solution of the material from Step A (0.24 g, 0.63 mmol) in dichloromethane (5 mL). After stirring overnight, another 0.5 mL of trifluoroacetic acid was added. After an additional 2 h, the reaction was concentrated. This material was dissolved in acetonitrile (5 mL) and carbonyldiimidazole (0.31 g, 1.89 mmol) was added at room temperature. After 2 h, the acetonitrile was evaporated in vacuo, the residue partitioned between 1N NaOH and dichloromethane, and the organic phase dried over magnesium sulfate. The crude product was purified by chromatography (silica gel, 10 to 15% methanol in methylene chloride gradient elution), which gave the title compound (0.089 g). MS 305.3.

1. waitAfter an additional 2 h
2. concentrationthe reaction was concentrated
3. dissolutionThis material was dissolved in acetonitrile (5 mL)
4. waitAfter 2 h
5. customthe acetonitrile was evaporated in vacuo
6. customthe residue partitioned between 1N NaOH and dichloromethane
7. dry with materialthe organic phase dried over magnesium sulfate
8. customThe crude product was purified by chromatography (silica gel, 10 to 15% methanol in methylene chloride gradient elution), which