C1(P(Cl)(Cl)(Cl)[Cl:8])C=CC=CC=1.[F:12][C:13]([F:40])([C:36]([F:39])([F:38])[F:37])[C:14]([F:35])([F:34])[C:15]([P:18]([C:21]([F:33])([F:32])[C:22]([F:31])([F:30])[C:23]([F:29])([F:28])[C:24]([F:27])([F:26])[F:25])(=O)[OH:19])([F:17])[F:16].Cl>>[F:12][C:13]([F:40])([C:36]([F:39])([F:38])[F:37])[C:14]([F:35])([F:34])[C:15]([P:18]([Cl:8])([C:21]([F:33])([F:32])[C:22]([F:31])([F:30])[C:23]([F:29])([F:28])[C:24]([F:27])([F:26])[F:25])=[O:19])([F:17])[F:16]Variant b) The mixture of 4.6 g (18.4 mmol) of phenyltetrachlorophosphorane and 7.3 g (14.5 mmol) of bis(nonafluorobutyl)phosphinic acid is stirred at room temperature for four hours When the evolution of gas (HCl) is complete, the nonafluorobutylphosphonyl dichloride is separated off by distillation at atmospheric pressure, giving 5.73 g of bis(nonafluorobutyl)phosphinyl chloride as colourless liquid substance. This corresponds to a yield of 76%, based on the phosphinic acid employed.
Loading…