反应详情

To a solution of the product from Step A (1.36 g, 5.6 mmol) in 20 mL of THF at 0° C. under Ar was added triphenylphosphine (1.8 g, 6.9 mmol), diethylazodicarboxylate (1.12 mL, 6.9 mmol) and diphenylphosphoryl azide (1.52 mL, 6.9 mmol). The ice-bath was removed and the reaction mixture was stirred at ambient temperature for 20 hours. The reaction was concentrated in vacuo and purified by silica gel chromatography (2% EtOAc/Hexane) to provide the desired product as a nearly colorless gum.

1. customThe ice-bath was removed
2. concentrationThe reaction was concentrated in vacuo
3. custompurified by silica gel chromatography (2% EtOAc/Hexane)