Acetylene → HCID 19601757, compound

Hydrosilation of acetylene with bis(dichlorosilyl)trichlorosilylmethane in the presence of H2PtCl6. To a 50 ml, three-necked, dried, flask equipped with a magnetic stirrer was added 200 μl of a 0.1 M H2PtCl6 /isopropyl alcohol (IPA) solution. The flask was placed under dry nitrogen atmosphere and the IPA removed under vacuum. Then, 6.29 g of bis(dichlorosilyl)trichlorosilylmethane and 25 ml of dried benzene were added to the flask forming a solution. The solution was maintained at reflux temperature and acetylene gas fed into the solution at a rate of 90 ml per minute for 10 hours. The resulting products were vacuum distilled at 67 Pa to yield 6.36 g of 1,1,3,3-tetrachloro-2-trichlorosilyl-1,3-disilacyclopent-4-ene (TCD-GC are 81.4%) (TCD-GC =gas chromatography using a thermal conductivity detector) and 1,1,3,3-tetrachloro-2-trichlorosilyl-1,3-disilacyclopentane (TCD-GC 4.2%) as a mixture. The structure of 1,1,3,3-tetrachloro-2-trichlorosilyl-1,3-disilacyclopent-4-ene was confirmed by 1H-NMR (CDCl3, ppm): 1.52 (s, 1H, SiCHSi), 7.42 (s, 2H, CH=CH).

1. customTo a 50 ml, three-necked, dried
2. customflask equipped with a magnetic stirrer
3. additionwas added 200 μl of a 0.1 M H2PtCl6 /isopropyl alcohol (IPA) solution
4. customthe IPA removed under vacuum
5. additionThen, 6.29 g of bis(dichlorosilyl)trichlorosilylmethane and 25 ml of dried benzene were added to the flask
6. customforming a solution
7. temperatureThe solution was maintained
8. distillationdistilled at 67 Pa

ORD record

ord-2863b678cc274116adb83d1dafb7414a

Source dataset

uspto-grants-1999_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05998649