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Tetravinylsilane → Tetrakis-(diphenylphosphinoethyl) silane

HRID 1633418
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HRID 1633418 반응식
[CH:1]([Si:3]([CH:8]=[CH2:9])([CH:6]=[CH2:7])[CH:4]=[CH2:5])=[CH2:2].[C:10]1([PH:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1>>[C:17]1([P:16]([CH2:2][CH2:1][Si:3]([CH2:8][CH2:9][P:16]([C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)([CH2:6][CH2:7][P:16]([C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH2:4][CH2:5][P:16]([C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)[C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 66188TetravinylsilaneHCID 70017Diphenylphosphine2회

생성물 1

HCID 54116395Tetrakis-(diphenylphosphinoethyl) silane수율 39.2%

실험 절차

A mixture of 27.2 g (0.2 mole) of tetravinyl silane and 149.5 g (0.804 mole) diphenylphosphine was reacted in a quartz pressure tube at 200° C. with u.v. light initiation until most of the diphenyl phosphine was converted. The hot, molten reaction mixture was added to 720 g of hot tuluene with stirring. The tetraadduct product precipitated from the solution as a white crystalline solid. The mixture was allowed to cool to ambient temperature and then filtered with suction. After washing with toluene and drying in vacuo, 84 g (47.7%) of crude product was obtained. This was recrystallized from 1200 ml of xylene to obtain 69 g of pure tetrakis-(diphenylphosphinoethyl) silane of mp. 198°-199° C.

후처리

  1. custom
was reacted in a quartz pressure tube at 200° C. with u.v
  • additionThe hot, molten reaction mixture was added to 720 g of hot tuluene
  • customThe tetraadduct product precipitated from the solution as a white crystalline solid
  • filtrationfiltered with suction
  • washAfter washing with toluene
  • customdrying in vacuo
  • custom84 g (47.7%) of crude product was obtained
  • customThis was recrystallized from 1200 ml of xylene
  • 출처 및 근거

    ORD 기록
    ord-86397bd224e94b74a3488e07fdb2695d
    출처 데이터셋
    uspto-grants-1984_10
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04480137

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