Chlorotrimethylsilane → 1,2-Difluoro-3-trimethylsilylbenzene

HRID 257685

반응식

HRID 257685 반응식
C([Li])CCC.[F:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[F:13].[CH3:14][Si:15]([CH3:18])([CH3:17])Cl.C1COCC1>CCCCCC.O>[F:6][C:7]1[C:8]([F:13])=[CH:9][CH:10]=[CH:11][C:12]=1[Si:15]([CH3:18])([CH3:17])[CH3:14]

참가 물질

7

반응물 4

HCID 6397ChlorotrimethylsilaneHCID 8028TetrahydrofuranHCID 97061,2-DifluorobenzeneHCID 178418339Butyllithium

생성물 1

HCID 108993711,2-Difluoro-3-trimethylsilylbenzene

시약·촉매·용매 2

HCID 962Water용매HCID 8058Hexane용매

실험 절차

12.5 ml of a 1.6-molar solution of n-butyllithium in hexane is added dropwise at 0° C. to a mixture of 0.02 mol of 1,2-difluorobenzene, 0.02 mol of trimethylchlorosilane and 25 ml of THF. After stirring at room temperature for 1.5 hours, the reaction mixture is poured into water, the phases are separated, and the aqueous phase is extracted with 2×50 ml of methylene chloride. Drying over magnesium sulfate, evaporation of the solvent and chromatography give the pure product.

후처리

  1. customthe phases are separated
  2. extractionthe aqueous phase is extracted with 2×50 ml of methylene chloride
  3. dry with materialDrying over magnesium sulfate, evaporation of the solvent and chromatography
  4. customgive the pure product

출처 및 근거

ORD 기록
ord-8afda83419114c30a43bb1c65f1f85f2
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05262556

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