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Water → (S)-(+)-2-Methylbutyl p-toluenesulfonate

HRID 1861581
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HRID 1861581 반응식
[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7](Cl)(=[O:9])=[O:8])=[CH:3][CH:2]=1.[CH3:12][C@@H:13]([CH2:16][CH3:17])[CH2:14][OH:15].O>ClCCl.C(N(CC)CC)C>[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7]([O:15][CH2:14][C@@H:13]([CH3:12])[CH2:16][CH3:17])(=[O:9])=[O:8])=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 962WaterHCID 73974-Toluenesulfonyl chlorideHCID 2723602(S)-2-methyl-1-butanol

생성물 1

HCID 113324(S)-(+)-2-Methylbutyl p-toluenesulfonate수율 89%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8471Triethylamine용매

실험 절차

To a ice-cooled solution of p-toluenesulphonyl chloride (9.53 g, 50 mmol), (S)-2-methylbutan-1-ol (4.41 g, 50 mmol) in absolute dichloromethane (200 ml), triethylamine (84 ml) was dropwise added. After complete addition and stirring for further 6 h at room temperature, the reaction mixture was poured into water (150 ml), the organic layer was separated and the aqueous phase was further extracted with dichloromethane (2×200 ml). The combined organic extracts were washed with HCl 1N (2×200 ml), with saturated NaCl solution (2×200 ml), dried over magnesium sulphate and evaporated under reduced pressure. The obtained slightly yellow oil was chromatographed on silica (diethylether/petroleumether: 1/3) to give (s)-2-methyl-butyl p-toluenesulphonate as a colourless oil (Yield: 10.0 g, 89%).

후처리

  1. additionwas dropwise added
  2. additionAfter complete addition
  3. customthe organic layer was separated
  4. extractionthe aqueous phase was further extracted with dichloromethane (2×200 ml)
  5. washThe combined organic extracts were washed with HCl 1N (2×200 ml), with saturated NaCl solution (2×200 ml)
  6. dry with materialdried over magnesium sulphate
  7. customevaporated under reduced pressure
  8. customThe obtained slightly yellow oil
  9. customwas chromatographed on silica (diethylether/petroleumether: 1/3)

출처 및 근거

ORD 기록
ord-efcbd2ff430b4b4ea7b9258da4f85fcd
출처 데이터셋
uspto-grants-2003_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06534135B1

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