反应详情

In a round bottom flask, 1 L (715 g, 6.38 mots) of 1-octene and 1.3 L (12.76 mols) of hypophosphorus acid (50% aqueous solution), 50 mL of tert-butyl perbenzoate, as initiator, and 1.7 L of 2-propanol as solvent are stirred at 80° C. for 7 h. The completed reaction mixture is combined with 2.0 L of water and 2.0 L of n-heptane. The mixture is separated and the organic phase is further washed with 1 L water. The water layer is further washed with 1 L of heptane and all the heptane layers are combined. This mixture is treated with 1 kg of anhydrous sodium sulfate and the solvent is evaporated to obtain 1.12 kg of crude n-octyl phosphinic acid with 85% purity (31P NMR).

1. customThe completed reaction mixture
2. customThe mixture is separated
3. washthe organic phase is further washed with 1 L water
4. washThe water layer is further washed with 1 L of heptane and all the heptane layers
5. additionThis mixture is treated with 1 kg of anhydrous sodium sulfate
6. customthe solvent is evaporated