反应详情

A mixture of 3-formyl-benzonitrile (10 g, 76.26 mmol), triethylamine (9.26 g, 91.05 mmol) and dimethyl-phosphite (10.91 g, 99.14 mmol) was stirred in ethyl acetate at room temperature for 2 hours. The solvent was evaporated and the residue was dissolved in ethyl acetate (50 ml), washed with a saturated ammonium chloride solution (1×50 ml), dried (Na2SO4) and the filtrate was evaporated affording the crude [(3-cyanophenyl-hydroxymethyl]-phosphonic acid dimethyl ester as a yellow solid (13.60 g, 56.43 mmol, 74%).

1. customThe solvent was evaporated
2. dissolutionthe residue was dissolved in ethyl acetate (50 ml)
3. washwashed with a saturated ammonium chloride solution (1×50 ml)
4. dry with materialdried (Na2SO4)
5. customthe filtrate was evaporated