反应详情

A stirred apparatus is initially charged with 150 g of ethanol, 65 g of water, 150 g (3.75 mol) of sodium hydroxide and 183 g (1.25 mol) of ethyl(2-cyanoethyl)-phosphinic acid (produced as in Example 5). The mixture was heated under reflux and reacted at that temperature for about 10 hours. Then water and the butanol were removed from the reaction mixture by distillation. Following the addition of a further 500 ml of water, the mixture was neutralized by addition of about 61 g (0.63 mol) of concentrated sulfuric acid. The water is then distilled off in vacuo. The residue is taken up in ethanol and the insoluble salts are filtered off. The solvent of the filtrate is removed in vacuo to obtain 234 g (89% of theory) of 3-(ethylhydroxyphosphinyl)propionic acid sodium salt as a solid material.

1. temperatureThe mixture was heated
2. temperatureunder reflux
3. customreacted at that temperature for about 10 hours
4. customThen water and the butanol were removed from the reaction mixture by distillation
5. additionthe addition of a further 500 ml of water
6. distillationThe water is then distilled off in vacuo
7. filtrationthe insoluble salts are filtered off
8. customThe solvent of the filtrate is removed in vacuo