Tetravinylsilane → Tetrakis-(diphenylphosphinoethyl) silane

HRID 1633418

反応式

HRID 1633418 の反応式
[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

参加物

3

反応物 2

HCID 66188TetravinylsilaneHCID 70017Diphenylphosphine2 回

生成物 1

HCID 54116395Tetrakis-(diphenylphosphinoethyl) silane収率 39.2%

実験手順

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.

後処理

  1. customwas reacted in a quartz pressure tube at 200° C. with u.v
  2. additionThe hot, molten reaction mixture was added to 720 g of hot tuluene
  3. customThe tetraadduct product precipitated from the solution as a white crystalline solid
  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

出典と根拠

ORDレコード
ord-86397bd224e94b74a3488e07fdb2695d
出典データセット
uspto-grants-1984_10
特許番号
US04480137

関連ノート

読み込み中…