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Benzamidine → HCID 136454423、化合物

HRID 1747788
ノート
印刷プレビュー

反応式

HRID 1747788 の反応式
O=[C:2]([C:9]1[N:13]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:12]=[CH:11][CH:10]=1)[CH2:3][C:4]([O:6]CC)=O.[C:20]1([C:26](=[NH:28])[NH2:27])[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>CN(C=O)C>[C:20]1([C:26]2[NH:28][C:4](=[O:6])[CH:3]=[C:2]([C:9]3[N:13]([C:14]4[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=4)[N:12]=[CH:11][CH:10]=3)[N:27]=2)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=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 2332BenzamidineHCID 89586101HCID 89586101、化合物

生成物 1

HCID 136454423HCID 136454423、化合物収率 27.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of ethyl 3-oxo-3-(1-phenyl-1H-pyrazol-5-yl)propanoate (300 mg) in DMF (10.0 mL) was added benzenecarboximidamide (139 mg) at room temperature. The reaction mixture was heated using a microwave reactor at 140° C. for 30 min. The reaction mixture was extracted with dichloromethane. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (dichloromethane/methanol) to give the title compound (100 mg).

後処理

  1. temperatureThe reaction mixture was heated
  2. customat 140° C.
  3. customfor 30 min
  4. extractionThe reaction mixture was extracted with dichloromethane
  5. washThe extract was washed with saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customthe solvent was evaporated under reduced pressure
  8. customThe residue was purified by silica gel column chromatography (dichloromethane/methanol)

出典と根拠

ORDレコード
ord-3c67aabb5f6747748a2e79b054b882cb
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09150588B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート