反应详情

温度

100 °C

564 g (6 mol) of ethylphosphonous acid (produced as in Example 1) are dissolved in 860 g of water and initially charged to a 5 l five-necked flask equipped with thermometer, reflux condenser, high-performance stirrer and dropping funnel. After heating the reaction mixture to 100° C., 371 g (7 mol) of acrylonitrile and 500 g of a 5% strength sodium peroxodisulfate solution (1.5 mol % based on acrylonitrile) are added dropwise at atmospheric pressure over 1 h. The water is then distilled off in vacuo. The residue is taken up in tetrahydrofuran and extracted. The insoluble salts are filtered off. The solvent of the filtrate is removed in vacuo and the residue is recrystallized from acetone to leave 732 g (83% of theory) of ethyl-(2-cyanoethyl)phosphinic acid as oil.

1. additioninitially charged to a 5 l five-necked flask
2. customequipped with thermometer
3. temperaturereflux condenser, high-performance stirrer
4. distillationThe water is then distilled off in vacuo
5. extractionextracted
6. filtrationThe insoluble salts are filtered off
7. customThe solvent of the filtrate is removed in vacuo
8. customthe residue is recrystallized from acetone