反应详情

To a stirred solution of 0.05 g of lithium hydroxide monohydrate in 7.7 ml of water, is added a solution of 4.37 g of ethyl 3-aminopropyl(di-n-propyloxymethyl)phosphinate in 16.2 ml of ethanol. A slight exothermic reaction ensues and the reaction mixture becomes cloudy. A further 2 ml of water are added and the clear solution stirred at room temperature for 5 days. After this time the mixture is concentrated in vacuo at 55° and the residue redissolved in water and extracted with 3×10 ml of dichloromethane. The aqueous layer is again evaporated to dryness and the residue dissolved in 20 ml of water and treated with 0.51 ml of 85% phosphoric acid. After stirring overnight, the solid is removed by filtration. Evaporation of the filtrate and crystallisation of the residue from ethanol/ether affords 3-aminopropyl(di-n-propyloxymethyl)phosphinic acid, m.p. 223°-225°, as a white solid.

1. customA slight exothermic reaction ensues
2. concentrationAfter this time the mixture is concentrated in vacuo at 55°
3. dissolutionthe residue redissolved in water
4. extractionextracted with 3×10 ml of dichloromethane
5. customThe aqueous layer is again evaporated to dryness
6. dissolutionthe residue dissolved in 20 ml of water
7. additiontreated with 0.51 ml of 85% phosphoric acid
8. stirringAfter stirring overnight
9. customthe solid is removed by filtration
10. customEvaporation of the filtrate and crystallisation of the residue from ethanol/ether