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4-But-2-ynyloxy-benzenesulfonyl chloride → 4-But-2-ynyloxybenzenesulfonyl fluoride

HRID 278344
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인쇄 미리보기

반응식

HRID 278344 반응식
[CH2:1]([O:5][C:6]1[CH:11]=[CH:10][C:9]([S:12](Cl)(=[O:14])=[O:13])=[CH:8][CH:7]=1)[C:2]#[C:3][CH3:4].[F-:16].[K+].[F-].[F-].[Ca+2]>>[CH2:1]([O:5][C:6]1[CH:11]=[CH:10][C:9]([S:12]([F:16])(=[O:14])=[O:13])=[CH:8][CH:7]=1)[C:2]#[C:3][CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 111959284-But-2-ynyloxy-benzenesulfonyl chlorideHCID 23699612Calcium;potassium;trifluoride

생성물 1

HCID 111955204-But-2-ynyloxybenzenesulfonyl fluoride수율 80.3%

실험 절차

To a solution of 4-but-2-ynyloxybenzenesulfonyl chloride (prepared from Example 30, step 4) (2.0 g, 8.18 mmol) in acetonitrle (10 ml) was added KF-CaF2 (2.85 g, 16.3 mmol) and the resulting mixture was stirred for 4 hours at room temperature. The reaction mixture was filtered and the filterate was concentrated. The crude product was dissolved in EtOAc and washed with water. The organic layer was dried over anhydrous Na2SO4 and the solvent was removed to obtain 1.5 g (80%) of the product as solid.

후처리

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe filterate was concentrated
  3. dissolutionThe crude product was dissolved in EtOAc
  4. washwashed with water
  5. dry with materialThe organic layer was dried over anhydrous Na2SO4
  6. customthe solvent was removed

출처 및 근거

ORD 기록
ord-62efb4c525574cd2adbb7c5d4b559db0
출처 데이터셋
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06358980B1

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