4-Chlorobenzenesulfonyl chloride → HCID 68950965、化合物

HRID 730234ノート

反応式

HRID 730234 の反応式
[N+:1]([C:4]1[CH:9]=[C:8]([C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)[CH:7]=[CH:6][C:5]=1[NH2:16])([O-:3])=[O:2].[Cl:17][C:18]1[CH:23]=[CH:22][C:21]([S:24](Cl)(=[O:26])=[O:25])=[CH:20][CH:19]=1>N1C=CC=CC=1.C(OCC)(=O)C>[Cl:17][C:18]1[CH:23]=[CH:22][C:21]([S:24]([NH:16][C:5]2[CH:6]=[CH:7][C:8]([C:10]3[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=3)=[CH:9][C:4]=2[N+:1]([O-:3])=[O:2])(=[O:26])=[O:25])=[CH:20][CH:19]=1

参加物

5

反応物 2

HCID 73984-Chlorobenzenesulfonyl chlorideHCID 10353230HCID 10353230、化合物

生成物 1

HCID 68950965HCID 68950965、化合物収率 40%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 2-nitro-4-pyridin-4-ylphenylamine (1 mmol) in pyridine (3 mL), 4-chloro-benzenesulfonyl chloride (1.2 mmol) was added and the resulting mixture was stirred at room temperature for 24 h. The reaction mixture was diluted with ethyl acetate (20 mL). The contents were washed with brine (25 mL), dried over sodium sulfate and concentrated under vacuum. The residue obtained was purified by column chromatography eluting with hexanes/ethyl acetate (1:1) then ethyl acetate to give 156 mg of 4-chloro-N-(2-nitro-4-pyridin-4-ylphenyl)benzene sulfonamide.

後処理

  1. washThe contents were washed with brine (25 mL)
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated under vacuum
  4. customThe residue obtained
  5. customwas purified by column chromatography
  6. washeluting with hexanes/ethyl acetate (1:1)

出典と根拠

ORDレコード
ord-4188ca5cb1eb47b0beb5f9c9f30521b5
出典データセット
uspto-grants-2009_09
特許番号
US07582673B2

反応ノート

読み込み中…