Acetylene → 1,1,3,3-Tetrachloro-1,3-disilacyclopent-4-ene

Hydrosilation of acetylene with bis(dichlorosilyl)methane in the presence of H2PtCl6 /PPh3. Into the same apparatus as described in Example 1 were placed 235 μl of 0.1 M H2PtCl6 /IPA, the flask was purged with dry nitrogen and the IPA removed under vacuum. Into the flask were added 10 g of bis(dichlorosilyl)methane, 235 μl of 0.1 M PPh3 /benzene solution, and 20 ml of dried benzene. Acetylene gas was blown into the flask content at a rate of 90 ml/min for 10 hours. The products were vacuum distilled at 67 Pa to yield a mixture comprising 8.35 g of 1,1,3,3-tetrachloro-1,3-disilacyclopent-4-ene (TCD-GC area 22.4%); 1,1,3,3-tetrachloro-1,3-disilacyclopentane (TCD-GC area 27.4%), and 1,1,3,3,6,6,8,8-octachloro-1,3,6,8-tetrasilaoctane (TCD-GC area 22.9%).

1. customthe flask was purged with dry nitrogen
2. customthe IPA removed under vacuum
3. additionInto the flask were added 10 g of bis(dichlorosilyl)methane, 235 μl of 0.1 M PPh3 /benzene solution, and 20 ml of dried benzene
4. distillationdistilled at 67 Pa

ORD record

ord-c29e2543e212405ab1c5a238e866fc6b

Source dataset

uspto-grants-1999_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05998649