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

HRID 610731
ノート
印刷プレビュー

反応式

HRID 610731 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>[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

4

反応物 2

HCID 10821Phenylacetylene2 回HCID 57370748Bisdichlorosilylmethane2 回

生成物 1

HCID 713760143,3,5,5-Tetrachloro-1-phenyl-3,5-disilapent-1-ene収率 5.5%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

Hydrosilation of phenylacetylene with bis(dichlorosilyl)methane in the presence of RhCl(PPh3)3. Into the same apparatus as described in Example 1 were added 0.99 g of bis(dichlorosilyl)methane, 0.102 g of RhCl(PPh3)3, and 20 ml of dried benzene. The flask content was heated to reflux and 0.52 ml of phenylacetylene was added over a 10 minute period. The flask content was refluxed, with stirring, for another 2 hours and then the solvent removed at atmospheric pressure. The products were vacuum distilled at 67 Pa to give a mixture comprising 0.9 g of 3,3,5,5-tetrachloro-1-phenyl-3,5-disilapent-1-ene (TCD-GC area 5.5%) and 3,3,5,5-tetrachloro-1,7-diphenyl-3,5-disilahepta-1,6-diene (TCD-GC area 66.5%).

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-668d04143ead4829be91172cd89e4c7f
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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