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Water → HCID 86644418、化合物

HRID 2194711
ノート
印刷プレビュー

反応式

HRID 2194711 の反応式
[CH:1]([C:3]1[CH:7]=[C:6]([NH:8][S:9]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)(=[O:11])=[O:10])[N:5]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:4]=1)=[O:2].[C:24](=O)([O-])[O-].[K+].[K+].IC.O>CN(C)C=O>[CH:1]([C:3]1[CH:7]=[C:6]([N:8]([CH3:24])[S:9]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)(=[O:11])=[O:10])[N:5]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[N:4]=1)=[O:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 86644417HCID 86644417、化合物

生成物 1

HCID 86644418HCID 86644418、化合物収率 86%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of N-(3-formyl-1-phenyl-1H-pyrazol-5-yl)benzenesulfonamide (331 mg) in N,N-dimethylformamide (5 mL) were added potassium carbonate (182 mg) and iodomethane (215 mg) at room temperature. After stirring at room temperature for 1 hr, the mixture was further stirred at 80° C. for 1 hr, and allowed to cool to room temperature. Water was added and the mixture was extracted with ethyl acetate. The extract was washed with water and saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent:hexane-ethyl acetate=7:1→3:1) to give the title compound as a pale-yellow amorphous (yield 297 mg, yield 86%).

後処理

  1. stirringthe mixture was further stirred at 80° C. for 1 hr
  2. temperatureto cool to room temperature
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed with water and saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (eluent:hexane-ethyl acetate=7:1→3:1)

出典と根拠

ORDレコード
ord-024a57c969e44e14b637982fc714801c
出典データセット
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08334301B2

反応ノート

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