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This and other phosphonochloridous esters were best prepared by the procedure of Steininger (Chem. Ber., 1962, 95, 2993) for the comproportionation of the corresponding phosphonous dichloride and phosphonite. Thus, a solution of diethyl p-anisylphosphonite (7.5 g, 36 mmol) in dry ether (20 mL) was added to a solution of p-anisylphosphonous dichloride (8.2 g, 36 mmol) in ether (75 mL) at 5° C. The solution was warmed to room temperature and stirred two hours, then concentrated and distilled (Kugelrohr) at 105°-110° C. (0.1 mmHg). Yield: 9.4 g (60%); IR (neat) 1595, 1500, 1255, 1095, 1025, 930, 824 cm-1 ; 1H NMR (CDCL3) δ 7.9-7.5 (n, 2 H), 8.1-7.8 (m, 2 H), 4.0 (m, 2 H), 3.82, (s, 3 H), 1.30 (t, J=7 Hz, 3 H); 31P NMR (CDCl3) δ 177.2 (ca. 90%).

1. concentrationconcentrated
2. distillationdistilled (Kugelrohr) at 105°-110° C. (0.1 mmHg)