反应详情

A mixture of 27.2 g (0.2 mole) of tetravinyl silane and 149.5 g (0.804 mole) diphenylphosphine was reacted in a quartz pressure tube at 200° C. with u.v. light initiation until most of the diphenyl phosphine was converted. The hot, molten reaction mixture was added to 720 g of hot tuluene with stirring. The tetraadduct product precipitated from the solution as a white crystalline solid. The mixture was allowed to cool to ambient temperature and then filtered with suction. After washing with toluene and drying in vacuo, 84 g (47.7%) of crude product was obtained. This was recrystallized from 1200 ml of xylene to obtain 69 g of pure tetrakis-(diphenylphosphinoethyl) silane of mp. 198°-199° C.

1. customwas reacted in a quartz pressure tube at 200° C. with u.v
2. additionThe hot, molten reaction mixture was added to 720 g of hot tuluene
3. customThe tetraadduct product precipitated from the solution as a white crystalline solid
4. filtrationfiltered with suction
5. washAfter washing with toluene
6. customdrying in vacuo
7. custom84 g (47.7%) of crude product was obtained
8. customThis was recrystallized from 1200 ml of xylene