Reaktion #697894

Reaktionsgleichung

acetylene

acetylene

bis(dichlorosilyl)trichlorosilylmethane

→

1,1,3,3-tetrachloro-2-trichlorosilyl-1,3-disilacyclopent-4-ene

Ausbeute 81.4%

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTo a 50 ml, three-necked, dried
2. 2
   Sonstigeflask equipped with a magnetic stirrer
3. 3
   workup.ADDITIONwas added 200 μl of a 0.1 M H2PtCl6 /isopropyl alcohol (IPA) solution
4. 4
   Sonstigethe IPA removed under vacuum
5. 5
   workup.ADDITIONThen, 6.29 g of bis(dichlorosilyl)trichlorosilylmethane and 25 ml of dried benzene were added to the flask
6. 6
   Sonstigeforming a solution
7. 7
   TemperaturThe solution was maintained
8. 8
   workup.DISTILLATIONdistilled at 67 Pa

Vorschrift

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).

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