反应详情

温度

65 °C

An 80 mL Fischer-Porter high pressure bottle was charged with tetramethyldisiloxane (10.0 g), toluene (10.0 g) and Wilkinson's catalyst ((PPh3)3RhCl, 40 ppm), stirred and brought to 60° C. The bottle was attached to a manifold and pressurized with isobutylene (25 psig) and maintained at 60-70° C. for 8 h. The pressure was vented, and the reaction was sampled for GC analysis; found residual tetramethyldisiloxane, M′MR product and MRMR byproduct (2:95:3). The resulting material was stripped under vacuum (approx. 150 mm Hg) at 40° C. to remove olefin and M′M′, then filtered with Celite to yield 21.3 g M′MR product/toluene solution, 94% GC purity. This product was found to have an Si—H content of 11 cc H2/g by gasiometric titration.

1. custombrought to 60° C
2. aliquotthe reaction was sampled for GC analysis
3. customwas stripped under vacuum (approx. 150 mm Hg) at 40° C.
4. customto remove olefin and M′M′,
5. filtrationthen filtered with Celite
6. customto yield 21.3 g M′MR product/toluene solution, 94% GC purity