반응 #2507812

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1,1,1,4,4-pentachloro-1,4-disilabutane

trivinylchlorosilane

1,1,1,4,4-pentachloro-1,4-disilabutane

1,1,1,4,4-pentachloro-1,4-disilabutane

→

tris(3,3,6,6,6-pentachloro-3,6-disilahexyl)chlorosilane

수율 66.0%

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후처리

1. 1
   기타Strong exothermic reaction
2. 2
   온도heat
3. 3
   기타the temperature of the solution below 130° C
4. 4
   workup.ADDITIONAfter addition
5. 5
   온도heat
6. 6
   workup.DISTILLATIONAfter that solution was distilled

실험 절차

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.

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