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2-Amino-5-methylbenzenesulfonamide → 2-[2-(4-Chloro-2-methoxy-phenyl)-ethenesulfonylamino]-5-methyl-benzenesulfonamide

HRID 2283362
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HRID 2283362 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]=[CH:9][S:10](Cl)(=[O:12])=[O:11])=[C:4]([O:14][CH3:15])[CH:3]=1.[NH2:16][C:17]1[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][C:18]=1[S:24]([NH2:27])(=[O:26])=[O:25]>N1C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]=[CH:9][S:10]([NH:16][C:17]2[CH:22]=[CH:21][C:20]([CH3:23])=[CH:19][C:18]=2[S:24]([NH2:27])(=[O:25])=[O:26])(=[O:12])=[O:11])=[C:4]([O:14][CH3:15])[CH:3]=1
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참가 물질

4

반응물 2

HCID 2455842-Amino-5-methylbenzenesulfonamideHCID 739930052-(4-Chloro-2-methoxyphenyl)-ethenesulfonyl chloride

생성물 1

HCID 687826342-[2-(4-Chloro-2-methoxy-phenyl)-ethenesulfonylamino]-5-methyl-benzenesulfonamide수율 54%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

2-(4-Chloro-2-methoxy-phenyl)-ethenesulfonyl chloride (0.50 g, 1.87 mmol) was added slowly to a solution of 2-amino-5-methyl-benzenesulfonamide (0.38 g, 2.05 mmol) in anhydrous pyridine (10 mL) and the reaction mixture was stirred for 18 hours at room temperature. The solvent was removed in vacuo and the residue was dissolved in ethyl acetate (30 mL). The organic phase was washed with 1 M hydrochloric acid and brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. Purification by column chromatography gave 0.42 g (54% yield) of the title compound.

후처리

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue was dissolved in ethyl acetate (30 mL)
  3. washThe organic phase was washed with 1 M hydrochloric acid and brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customPurification by column chromatography

출처 및 근거

ORD 기록
ord-55df97f10b5d466da5ed2aaefe123d3a
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09145380B2

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