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Benzene → 3,3,5,5-Tetrachloro-1-phenyl-3,5-disilapent-1-ene

HRID 610729
ノート
印刷プレビュー

反応式

HRID 610729 の反応式
[C:1]1([C:7]#[CH:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl:9][SiH:10]([CH2:12][SiH:13]([Cl:15])[Cl:14])[Cl:11].C1C=CC=CC=1>O1CCCC1>[Cl:9][Si:10]([Cl:11])([CH2:12][SiH:13]([Cl:15])[Cl:14])[CH:8]=[CH:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 241BenzeneHCID 10821Phenylacetylene2 回HCID 57370748Bisdichlorosilylmethane2 回

生成物 1

HCID 713760143,3,5,5-Tetrachloro-1-phenyl-3,5-disilapent-1-ene収率 27.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Hydrosilation of phenylacetylene with bis(dichlorosilyl)methane in the presence of H2PtCl6 /THF. Into the same apparatus as described in Example 1 were added 1 g of bis(dichlorosilyl)methane, 20 μl of 0.1 M H2PtCl6 in THF (tetrahydrofuran) solution, and 20 ml of dried benzene. The flask content was heated to reflux and 0.52 ml of phenylacetylene was added over a ten minute period. The flask content was refluxed, with stirring, for another 8 hours and then the solvent removed at atmospheric pressure. The products were vacuum distilled at 67 Pa to give a mixture comprising 1.66 g of 3,3,5,5-tetrachloro-1-phenyl-3,5-disilapenta-1-ene (TCD-GC area 27.3%) and 3,3,5,5-tetrachloro-1,7-diphenyl-3,5-disilahepta-1,6-diene (TCD-GC area 26.4%).

後処理

  1. temperatureThe flask content was heated
  2. temperatureto reflux
  3. temperatureThe flask content was refluxed
  4. customthe solvent removed at atmospheric pressure
  5. distillationdistilled at 67 Pa

出典と根拠

ORDレコード
ord-4de2b1b3a328468aaa621dca56360a30
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05998649

反応ノート

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