反应详情

A suspension of 8.0 g of sodium hydride (55% dispersion in oil) in 35 ml of anhydrous tetrahydrofuran under an inert atmosphere is treated with 35 ml of an anhydrous tetrahydrofuran solution of 25 g of ethyl n-butylphosphinate. The resulting suspension is stirred at room temperature for 1 hour before dropwise addition of 32 ml of methyl iodide. After 3 hours stirring at room temperature 10 ml of water are carefully added followed by 200 ml of dichloromethane. Separation of the organic layer, drying over anhydrous magnesium sulphate and removal of the solvent in vacuo affords an oil. Kugelrohrdistillation at 90° and 10-1 mbar affords ethyl n-butyl-(methyl)phosphinate.

1. additionare carefully added
2. customSeparation of the organic layer
3. dry with materialdrying over anhydrous magnesium sulphate and removal of the solvent in vacuo
4. customaffords an oil