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Ethyl Acetate → (4-Triisopropylsilanylsulfanyl-phenyl)-methanol

HRID 2222941
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HRID 2222941 반응식
[CH:1]([Si:4]([SH:11])([CH:8]([CH3:10])[CH3:9])[CH:5]([CH3:7])[CH3:6])([CH3:3])[CH3:2].[H-].[K+].Br[C:15]1[CH:22]=[CH:21][C:18]([CH2:19][OH:20])=[CH:17][CH:16]=1.C(OCC)(=O)C>O1CCCC1.C1C=CC=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.[Pd]>[CH:1]([Si:4]([S:11][C:15]1[CH:22]=[CH:21][C:18]([CH2:19][OH:20])=[CH:17][CH:16]=1)([CH:5]([CH3:7])[CH3:6])[CH:8]([CH3:10])[CH3:9])([CH3:3])[CH3:2]
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참가 물질

8

반응물 4

HCID 8857Ethyl AcetateHCID 701194-Bromobenzyl alcoholHCID 82127Potassium hydrideHCID 3435097Tris(propan-2-yl)silanethiol

생성물 1

HCID 69114972(4-Triisopropylsilanylsulfanyl-phenyl)-methanol

시약·촉매·용매 3

HCID 11979704
Tetrakis(triphenylphosphine)palladium
촉매
HCID 241Benzene용매
HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of triisopropylsilyl thiol (1.904 g, 10.0 mmol) in tetrahydrofuran (10 mL) was added to a stirred suspension of potassium hydride in tetrahydrofuran (10 mL). The resulting suspension was then added to a stirred solution of 4-bromobenzyl alcohol (1.87 g, 10 mmol) and tetrakis[triphenylphosphine]palladium(0) (0.350 g, 0.30 mmol) in benzene (25 mL). The reaction mixture was stirred at reflux for 2 h under a nitrogen atmosphere. Ethyl acetate (200 mL) was added and the solution washed with water. The organic phase was dried with magnesium sulfate, filtered, and concentrated by rotary evaporation. The crude product was purified by silica gel chromatography using a gradient of 0% to 2% ethyl acetate in dichloromethane to yield (4-triisopropylsilanylsulfanyl-phenyl)-methanol as a colorless oil.

후처리

  1. temperatureat reflux for 2 h under a nitrogen atmosphere
  2. washthe solution washed with water
  3. dry with materialThe organic phase was dried with magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated by rotary evaporation
  6. customThe crude product was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-b0de1392b0b84d2185cf6f1d50ed2ab3
출처 데이터셋
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07371747B2

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