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Chlorotrimethylsilane → Silane, (4-bromophenyl)trimethyl-

HRID 64621
ノート
印刷プレビュー

反応式

HRID 64621 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5](Br)=[CH:4][CH:3]=1.C([Li])CCC.[CH3:14][Si:15]([CH3:18])([CH3:17])Cl>CCOCC.CCCCCC>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([Si:15]([CH3:18])([CH3:17])[CH3:14])=[CH:4][CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6397ChlorotrimethylsilaneHCID 78041,4-DibromobenzeneHCID 178418339Butyllithium

生成物 1

HCID 138897Silane, (4-bromophenyl)trimethyl-

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回HCID 8058Hexane溶媒

実験手順

Under argon, 94.4 g of p-dibromobenzene is cooled to -20° C. in 400 ml of absolute ether. To the solution is added dropwise 255 ml of 15% butyllithium in hexane so that the temperature does not rise above -10° C. Then the mixture is agitated for one hour at room temperature. After a negative Gilman test (H. Gilman, J. Swiss, J. Amer. Chem. Soc. 62: 1847 [1940]), the mixture is again cooled to -20° C. and 46 ml of trimethylchlorosilane in 200 ml of absolute ether is added dropwise thereto so that the temperature does not exceed -10° C. After the addition step is finished, the mixture is stirred for 16 hours at room temperature and another hour under reflux. The thus-formed precipitate is suctioned off and thoroughly washed with ether. The resultant filtrate is concentrated and then distilled with a water-jet aspirator, thus producing 65.52 g of p-bromotrimethylsilylbenzene, bp (16 torr) 103°-110° C.

後処理

  1. customdoes not rise above -10° C
  2. temperatureAfter a negative Gilman test (H. Gilman, J. Swiss, J. Amer. Chem. Soc. 62: 1847 [1940]), the mixture is again cooled to -20° C.
  3. customdoes not exceed -10° C
  4. additionAfter the addition step
  5. stirringthe mixture is stirred for 16 hours at room temperature and another hour
  6. temperatureunder reflux
  7. washthoroughly washed with ether
  8. concentrationThe resultant filtrate is concentrated
  9. distillationdistilled with a water-jet aspirator

出典と根拠

ORDレコード
ord-380ef2b45f9e43889dd62b604dbfb785
出典データセット
uspto-grants-1986_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04609651

反応ノート

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