Tetravinylsilane → Tetrakis-(diphenylphosphinoethyl) silane

HRID 544516

반응식

HRID 544516 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>C1(C)C=CC=CC=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 물질

4

반응물 2

HCID 66188TetravinylsilaneHCID 70017Diphenylphosphine2회

생성물 1

HCID 54116395Tetrakis-(diphenylphosphinoethyl) silane수율 39.2%

시약·촉매·용매 1

HCID 1140Toluene용매

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 720g of hot toluene with stirring. The tetraaduct product precipitated from the solution as a white crystalline solid. The mixture was allowed to coolto 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 the pure tetrakis-(diphenylphosphinoethyl) silane of mp. 198°-199° C.

후처리

  1. customwas reacted in a quartz pressure tube at 200° C. with u.v
  2. customThe tetraaduct product precipitated from the solution as a white crystalline solid
  3. customto coolto ambient temperature
  4. filtrationfiltered with suction
  5. washAfter washing with toluene
  6. customdrying in vacuo
  7. custom84 g (47.7%) of crude product was obtained
  8. customThis was recrystallized from 1200 ml of xylene

출처 및 근거

ORD 기록
ord-1d831e6dd0de40a7b7c4844939fec56f
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04450299

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