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

HRID 2283362
ノート
印刷プレビュー

反応式

HRID 2283362 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-55df97f10b5d466da5ed2aaefe123d3a
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09145380B2

反応ノート

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