5-Bromo-2-methoxybenzene-1-sulfonyl chloride → HCID 11614188、化合物

HRID 730236ノート

反応式

HRID 730236 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=2)[CH:5]=[CH:4][C:3]=1[NH:14][S:15]([C:18]1[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][CH:19]=1)(=[O:17])=[O:16].[Br:25][C:26]1[CH:27]=[CH:28][C:29]([O:36][CH3:37])=[C:30]([S:32](Cl)(=[O:34])=[O:33])[CH:31]=1>N1C=CC=CC=1.C(OCC)(=O)C>[Br:25][C:26]1[CH:27]=[CH:28][C:29]([O:36][CH3:37])=[C:30]([S:32]([NH:1][C:2]2[CH:7]=[C:6]([C:8]3[CH:9]=[CH:10][N:11]=[CH:12][CH:13]=3)[CH:5]=[CH:4][C:3]=2[NH:14][S:15]([C:18]2[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][CH:19]=2)(=[O:16])=[O:17])(=[O:33])=[O:34])[CH:31]=1

参加物

5

反応物 2

HCID 5200205-Bromo-2-methoxybenzene-1-sulfonyl chlorideHCID 68950992HCID 68950992、化合物

生成物 1

HCID 11614188HCID 11614188、化合物収率 80.5%

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of N-(2-amino-4-pyridin-4-ylphenyl)-4-chlorobenzene sulfonamide (0.1 mmol) in pyridine (0.5 mL), 5-bromo-2-methoxy-benzenesulfonyl chloride (0.12 mmol) was added. The reaction mixture was stirred at room temperature for 2 h and then was diluted with ethyl acetate (10 mL). The contents were washed with brine (10 mL), dried over sodium sulfate, and concentrated under vacuum. The residue obtained was purified by column chromatography eluting with hexanes/ethyl acetate (1:1) followed by ethyl acetate to give 49 mg of 5-bromo-N-[2-(4-chlorobenzenesulfonylamino) -5-pyridin-4-ylphenyl]-2-methoxybenzenesulfonamide. LC: Tr 0.94 min, MS: 610.8 (M+1)+.

後処理

  1. washThe contents were washed with brine (10 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-1adc025a969044bbbdd2eba7f554eb48
出典データセット
uspto-grants-2009_09
特許番号
US07582673B2

反応ノート

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