反应详情

A mixture of 6.6 g of hypophosphorous acid (95% solution in water) and 86 g of tri-n-propyl orthoformate is treated with 0.77 ml of trifluoracetic acid. The two-phase mixture is stirred at room temperature for 48-72 hours until the reaction is complete. This can be monitored by 31P-NMR or thin layer chromatography. The reaction mixture is diluted with 200 ml of dichloromethane and washed twice with 150 ml of a saturated aqueous solution of sodium bicarbonate. After drying the dichloromethane layer over anhydrous magnesium sulphate and removal of the solvent in vacuo, a colorless oil is obtained which after distillation affords di-n-propyloxymethylphosphonous acid n-propyl ester, b.p. 45°/2×104 mbar.

1. washwashed twice with 150 ml of a saturated aqueous solution of sodium bicarbonate
2. dry with materialAfter drying the dichloromethane layer
3. customover anhydrous magnesium sulphate and removal of the solvent in vacuo
4. customa colorless oil is obtained which
5. distillationafter distillation