反应详情

Di[p-(3-phenylpropyl)phenyl]chlorophosphine 1 (6.0 g, 13.1 mmol) was dissolved in 150 ml THF and Li (0.185 g, 26.2 mmol) was chopped directly into the reaction flask under Ar. A deep red solution was resulted in 10 min and all the lithium was consumed in 4 h. The solvent was removed by vacuum and 100 ml diethyl ether was added. The organic phase was washed 3×20 ml H2O and dried over MgSO4. Ether was then removed by vacuum and the final product was obtained as a pale yellow oil with quantitative yield. 2 was characterized by 31P NMR. -42.5, 'JH-P =211 Hz.

1. customA deep red solution was resulted in 10 min
2. customall the lithium was consumed in 4 h
3. customThe solvent was removed by vacuum and 100 ml diethyl ether
4. additionwas added
5. washThe organic phase was washed 3×20 ml H2O
6. dry with materialdried over MgSO4
7. customEther was then removed by vacuum