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4-Fluorobenzenesulfonyl chloride → 4-fluoro-N,N-dimethylbenzenesulfonamide

HRID 238586
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HRID 238586 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8](Cl)(=[O:10])=[O:9])=[CH:4][CH:3]=1.Cl.[CH3:13][NH:14][CH3:15]>O1CCCC1.CN(C)C1C=CN=CC=1>[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:14]([CH3:15])[CH3:13])(=[O:10])=[O:9])=[CH:4][CH:3]=1
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참가 물질

5

반응물 2

HCID 95884-Fluorobenzenesulfonyl chlorideHCID 10473Dimethylamine, hydrochloride

생성물 1

HCID 7993014-fluoro-N,N-dimethylbenzenesulfonamide수율 50.2%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 4-fluorobenzenesulfonyl chloride (1.95 g, 10 mmol) and dimethylamine hydrochloric acid salt (978 mg, 12 mmol) in tetrahydrofuran (10 mL) was added to a solution of 4-dimethylaminopyridine (3.05 g, 25 mmol) in tetrahydrofuran (10 mL) dropwise at room temperature. The resulting mixture was stirred at room temperature overnight and concentrated in vacuo. The residue was purified by flash column (elution with 20% ethyl acetate in petroleum ether) to afford 4-fluoro-N,N-dimethyl-benzenesulfonamide (1.02 g, 50%) as a white solid.

후처리

  1. concentrationconcentrated in vacuo
  2. customThe residue was purified by flash column (elution with 20% ethyl acetate in petroleum ether)

출처 및 근거

ORD 기록
ord-c34f281a33e1453d9f9dfb56f45d63b8
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08642629B2

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