反应 #3352035
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05064819
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 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. washed twice with 150 ml of a saturated aqueous solution of sodium bicarbonate over anhydrous magnesium sulphate and removal of the solvent in vacuo a colorless oil is obtained which after distillation
来源 ID: ord-c411e3e174b3456ab9a6a6900bd7599b