[C:1]1([P:7](Cl)Cl)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:10]([OH:12])[CH3:11].N1C=CC=CC=1.[OH2:19]>CCOCC>[C:1]1([PH:7](=[O:19])[O:12][CH2:10][CH3:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1A solution of phenylphosphonous dichloride (66 g, 0.37 mol) in dry ether (100 mL) was treated dropwise with a solution of ethanol (21.6 mL, 0.37 mol) and pyridine (29.6 mL, 0.37 mol) in ether (200 mL) at room temperature under argon. After stirring for one hour, a mixture of water (6.6 mL, 0.37 mol) and pyridine (29.6 mL) was added slowly. The reaction mixture was filtered, washed with ether, and the ether evaporated to give an oil. The oil was distilled in the Kugelrohr and then through a short Vigreux column at 95°-98° C. (0.05 mmHg); lit. (T. L. Emmick et al., J. Am. Chem. Soc., 1968, 90, 3459) 102°-103° C. (0.2 mmHg). Yield 44.3 g (70%). 1H NMR (CDCl3)δ7.57 (d, J=569 Hz, 1H), 8.0-7.4 (m, 5H), 4.13 (2 q, JH-H =7 Hz, JP-H =14 Hz, 2H), 1.35 (t, J=7 Hz, 3H).
Wird geladen…
