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Dichlorodimethylsilane → HCID 178427960, 화합물

HRID 585176
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HRID 585176 반응식
[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
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참가 물질

6

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HCID 6398DichlorodimethylsilaneHCID 5755861H-Indene, 2-bromo-HCID 5462224Magnesium2회HCID 178504339HCID 178504339, 화합물

생성물 1

HCID 178427960HCID 178427960, 화합물수율 94%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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 After stirring, solvent was withdrawn and 50 ml of THF was newly added.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%).

후처리

  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 customsolvent was withdrawn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

출처 및 근거

ORD 기록
ord-1c779a3f7f554fe7ad7f9bc17d99f7b1
출처 데이터셋
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06930160B2

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