反应详情

A mixture of 34.4 g (0.25 moles) of PCl3 in 400 mL of hexane was treated with Cy2NH (90.7 g, 0.50 moles) dropwise at ° C. for 30 min. The resulting white slurry was warmed to room temperature and stirred for 1 h, refluxed overnight before removal of Cy2NH—HCl by filtration. The white solids were washed with hexane (2×100 mL). The combined filtrates were concentrated to give the crude Cy2N—PCl2 (54.0 g, 77% yield). 31P NMR (121 MHz, CD2Cl2): δ171.3 (s) ppm.

1. washThe white solids were washed with hexane (2×100 mL)
2. concentrationThe combined filtrates were concentrated