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 driving 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. customover anhydrous magnesium sulphate and removal of the solvent in vacuo
3. customa colorless oil is obtained which
4. distillationafter distillation