反应详情

A solution of diethoxymethylphosphinic acid ethyl ester is added within a period of 90 minutes, under argon, to a suspension of 13.2 g of 99% sodium hydride in 500 ml of tetrahydrofuran, the temperature being maintained at 20°. The reaction is exothermic and is accompanied by the evolution of gas. The mixture is then stirred for 90 minutes, and 85.5 g of benzyl bromide are then added within a period of 20 minutes. The mixture is then stirred at room temperature for 24 hours and cooled to 0°, and 100 ml of water are added carefully. The organic solvents are removed under reduced pressure and the residue is partitioned between water and dichloromethane. The organic phase is separated off, washed with water, dried over sodium sulfate and concentrated by evaporation. Distillation of the residue under reduced pressure yields diethoxymethyl(benzyl)phosphinic acid ethyl ester having a boiling point of 103°-110° (3×10-4 bar).

1. temperaturethe temperature being maintained at 20°
2. stirringThe mixture is then stirred at room temperature for 24 hours
3. temperaturecooled to 0°
4. customThe organic solvents are removed under reduced pressure
5. customthe residue is partitioned between water and dichloromethane
6. customThe organic phase is separated off
7. washwashed with water
8. dry with materialdried over sodium sulfate
9. concentrationconcentrated by evaporation
10. distillationDistillation of the residue under reduced pressure