反应详情

温度

130 °C

A magnetically stirred mixture of 15.6 g (0.06 mole) of i-butyl bis-(dimethylaminopropyl) phosphine of Example 10 and 12.3 g (0.06 mole) of n-dodecyl chloride was heated under nitrogen to 130° C. and then kept there for 24 hours. The nmr spectrum of a sample of the heated mixture showed a substantial selective quaternarization of the t-phosphine moiety. Accordingly, the crude mixture was heated at 150° C. at 0.2 mm. to distill off the volatile unreacted compounds and to obtain the residual product, i.e. bis-(3-dimethylaminopropyl) dodecyl i-butyl phosphonium chloride. The product weighed 23 g, 82% of the calculated yield, and hardened to a wax like solid at room temperature. Nmr indicated that quaternarization occurred at the phosphine group.

1. distillationto distill off the volatile unreacted compounds