反应详情

Diethyl benzylphosphonate (5.0 mL, 5.5 g, 24 mmol) was dissolved in absolute EtOH (25 mL), then 50% NaOH (3 mL) was added. The reaction was heated under reflux overnight, allowed to cool to RT, then partitioned between 2N HCl and EtOAc. Washed organic layer with brine, extracted combined aqueous layers with EtOAc, dried combined organic layers over Na2SO4. After filtration and concentration recovered 4.5 g (93%). MS (DCI/NH3) 201/218 (M+H)+/(M+H+NH3)+.

1. temperatureThe reaction was heated
2. temperatureunder reflux overnight
3. custompartitioned between 2N HCl and EtOAc
4. extractionWashed organic layer with brine, extracted
5. customdried
6. filtrationAfter filtration and concentration
7. customrecovered 4.5 g (93%)