反应详情

To a solution of 20.9 g (64.5 mmol) of the azido compound obtained in Step B in 650 mL of THF, there are successively added 25.5 g (97.2 mmol) of triphenylphosphine and 157 mL of water. The batch is refluxed for 2 hours 30 minutes. The reaction mixture is then concentrated to dryness and the residue oil is then taken up in isopropyl ether. A white precipitate appears; it is filtered off and washed with isopropyl ether. The filtrate is then concentrated to dryness and then purified by chromatography over silica gel using dichloromethane and methanol as eluants. The title product is obtained in the form of an oil.

1. temperatureThe batch is refluxed for 2 hours 30 minutes
2. concentrationThe reaction mixture is then concentrated to dryness
3. filtrationit is filtered off
4. washwashed with isopropyl ether
5. concentrationThe filtrate is then concentrated to dryness
6. custompurified by chromatography over silica gel