[CH2:1]([P:3]([OH:5])[OH:4])[CH3:2].[C:6](#[N:9])[CH:7]=[CH2:8].[O-]S(OOS([O-])(=O)=O)(=O)=O.[Na+].[Na+]>O>[CH2:1]([P:3]([CH2:8][CH2:7][C:6]#[N:9])(=[O:5])[OH:4])[CH3:2]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-neck flask equipped with thermometer, reflux condenser, high-performance stirrer and dropping funnel. The reaction mixture is heated to 100° C. and 371 g (7 mol) of acrylonitrile and 500 g of a 5% sodium peroxodisulfate solution (1.5 mol % based on acrylonitrile) are added dropwise at atmospheric pressure. Then, the water is distilled off, and the residue is taken up in THF, extracted and filtered. The solvent of the filtrate is removed in vacuo to leave 732 g (83% of theory) of ethyl(2-cyanoethyl)phosphinic acid as oil.
Wird geladen…
