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Dichlorodimethylsilane → HCID 178427960、化合物

HRID 585176
ノート
印刷プレビュー

反応式

HRID 585176 の反応式
[Mg].[Cl:2][C:3]1[CH:4]([SiH](C)C)[C:5]2[C:10]([CH:11]=1)=[CH:9][CH:8]=[CH:7][CH:6]=2.Br[C:16]1CC2C(C=1)=CC=CC=2.Cl[Si:26](Cl)([CH3:28])C>O1CCCC1>[Cl:2][C:3]1[CH:28]([SiH3:26])[C:6]2[C:5]([C:4]=1[CH3:16])=[C:10]([CH3:11])[CH:9]=[CH:8][CH:7]=2
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 6398DichlorodimethylsilaneHCID 5755861H-Indene, 2-bromo-HCID 5462224Magnesium2 回HCID 178504339HCID 178504339、化合物

生成物 1

HCID 178427960HCID 178427960、化合物収率 94%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Under nitrogen flow, 50 ml of THF (tetrahydrofuran) and 2.5 g (41 mmol) of magnesium was placed in a 1 liter 3-necked flask, to which 0.1 ml of 1 2-dibromoethane was added and stirred for 30 minutes to activate magnesium. After stirring, solvent was withdrawn and 50 ml of THF was newly added. To this, 5.0 g (25.6 mmol) of 2-bromoindene in THE (200 ml) solution was dropped in 2 hours. Then the solution was stirred at room temperature for 2 hours and cooled down to −78 ° C., to which 3.1 ml (25.6 mmol) of dichlorodimethylsilane in THF (100 ml) solution was dropped in one hour, followed by stirring for 15 hours and the solvent was distilled off. The residue was extracted by 200 ml of hexane and by distilling off the solvent, 6.6 g (24.2 mmol) of 2-chloro-dimethyl-silylindene was obtained (yield 94%).

後処理

  1. additionwas added
  2. stirringAfter stirring
  3. customsolvent was withdrawn
  4. addition50 ml of THF was newly added
  5. stirringThen the solution was stirred at room temperature for 2 hours
  6. additionwas dropped in one hour
  7. stirringby stirring for 15 hours
  8. distillationthe solvent was distilled off
  9. extractionThe residue was extracted by 200 ml of hexane
  10. distillationby distilling off the solvent

出典と根拠

ORDレコード
ord-1c779a3f7f554fe7ad7f9bc17d99f7b1
出典データセット
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06930160B2

反応ノート

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