反应详情

Hydrolysis of Dibutyl Carboxyethylmethylphosphinate 528 g (2 mol) of the dibutyl carboxyethylmethylphosphinate obtained according to Example 4 are charged to a 1 l five-neck flask fitted with thermometer, reflux condenser, high-speed stirrer and dropping funnel. At 160° C., 500 ml of water are metered in over 4 h and a butanol-water mixture is distilled off. 281 g of butanol are obtained, which corresponds to 95% of theory. The distillatively removed butanol is re-used to esterify the methylphosphonous acid. 300 g of carboxyethylmethylphosphinic acid are obtained as a white solid having a melting point of about 95° C. and a 31P NMR purity of >97%.

1. customobtained
2. additionare charged to a 1 l five-neck flask
3. customfitted with thermometer
4. temperaturereflux condenser, high-speed stirrer
5. customAt 160° C.
6. customare metered in over 4 h
7. distillationa butanol-water mixture is distilled off
8. custom281 g of butanol are obtained