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Phenylacetylene → Silanediamine, N,N,N',N'-tetraethyl-1,1-bis(phenylethynyl)-

HRID 612975
ノート
印刷プレビュー

反応式

HRID 612975 の反応式
[CH2:1]([Li])[CH2:2][CH2:3][CH3:4].[C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)#[CH:7].Cl[Si:15](Cl)([N:21]([CH2:24][CH3:25])[CH2:22][CH3:23])[N:16]([CH2:19][CH3:20])[CH2:17][CH3:18].[Cu](C#N)C#N>O1CCCC1>[CH2:17]([N:16]([Si:15]([N:21]([CH2:24][CH3:25])[CH2:22][CH3:23])([C:7]#[C:6][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:1]#[C:2][C:3]1[CH:4]=[CH:4][CH:3]=[CH:2][CH:1]=1)[CH2:19][CH3:20])[CH3:18]
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 4

HCID 10821PhenylacetyleneHCID 131337371,1-Dichloro-N,N,N',N'-tetraethylsilanediamineHCID 178418260HCID 178418260、化合物HCID 178418339Butyllithium

生成物 1

HCID 11760549Silanediamine, N,N,N',N'-tetraethyl-1,1-bis(phenylethynyl)-収率 93%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

1.6 N normal butyl lithium 205 ml was dropwise added to a solution comprising 33 ml of ethynylbenzene and 300 ml of tetrahydrofuran (hereinafter abbreviated as THF) at 0° C. under nitrogen gas flow, and stirring was continued for 1.5 hour. Dichlorobis(diethylamino)silane 36.5 g and 672 mg of copper cyanide were added to the resulting solution, and stirring was continued at room temperatures for 20 minutes to carry out the reaction. Solid matters precipitated in the reaction liquid were removed by filtering, and then the filtrate was concentrated. Water was added to this concentrate to extract the product with ether. This ether extraction layer was washed with water and then dried on magnesium sulfate. An ether component of this liquid was distilled off, and then the residue was refined by distillation to obtain 52 g of bis(diethylamino)-bis(phenyethynyl)silane. The yield was 93%.

後処理

  1. customat 0° C.
  2. stirringstirring
  3. waitwas continued at room temperatures for 20 minutes
  4. customthe reaction
  5. customSolid matters precipitated in the reaction liquid
  6. customwere removed
  7. filtrationby filtering
  8. concentrationthe filtrate was concentrated
  9. additionWater was added to
  10. concentrationthis concentrate
  11. extractionto extract the product with ether
  12. extractionThis ether extraction layer
  13. washwas washed with water
  14. customdried on magnesium sulfate
  15. distillationAn ether component of this liquid was distilled off
  16. distillationthe residue was refined by distillation

出典と根拠

ORDレコード
ord-a18b6cfd517f4267828a5bcf84c851cf
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06005128

反応ノート

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