反応 #2507812

ord-4d8d3d9d33704160a92dbd9b1a29d2a4

反応方程式

Cl[SiH](Cl)CC[Si](Cl)(Cl)Cl
1,1,1,4,4-pentachloro-1,4-disilabutane
C=C[Si](Cl)(C=C)C=C
trivinylchlorosilane
Cl[SiH](Cl)CC[Si](Cl)(Cl)Cl
1,1,1,4,4-pentachloro-1,4-disilabutane
Cl[SiH](Cl)CC[Si](Cl)(Cl)Cl
1,1,1,4,4-pentachloro-1,4-disilabutane
Cl[Si](Cl)(Cl)CC[Si](Cl)(Cl)CC[Si](Cl)(CC[Si](Cl)(Cl)CC[Si](Cl)(Cl)Cl)CC[Si](Cl)(Cl)CC[Si](Cl)(Cl)Cl
tris(3,3,6,6,6-pentachloro-3,6-disilahexyl)chlorosilane
収率 66.0%

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他Strong exothermic reaction
  2. 2
    温度heat
  3. 3
    その他the temperature of the solution below 130° C
  4. 4
    workup.ADDITIONAfter addition
  5. 5
    温度heat
  6. 6
    workup.DISTILLATIONAfter that solution was distilled

実験手順

11.00 g (0.076 mol) trivinylchlorosilane was added to a 100 ml vessel followed by 2 ml 1,1,1,4,4-pentachloro-1,4-disilabutane. The solution was heated to 80° C. and 15 μL of a 10% H2PtCl6/IPA-solution was added. Strong exothermic reaction was observed and heat was switched off. Rest of 1,1,1,4,4-pentachloro-1,4-disilabutane was added slowly during 30 min keeping the temperature of the solution below 130° C. The total amount of 1,1,1,4,4-pentachloro-1,4-disilabutane was 61.50 g (0.234 mol, 2.6% excess). After addition heat was again switched on and solution was stirred for an hour at 110° C. After that solution was distilled yielding 47.08 g (66%) tris(3,3,6,6,6-pentachloro-3,6-disilahexyl)chlorosilane. B.p. 264° C./<0.5 mbar.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07955660B2uspto-grants-2011_06