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Ammonium Acetate → (1,4-bis-(4-fluoro-phenyl)-1H-imidazol-2-yl)-acetic acid ethyl ester

HRID 1428941
ノート
印刷プレビュー

反応式

HRID 1428941 の反応式
[CH2:1]([O:3][C:4](=[O:26])[CH2:5][C:6]([N:8]([C:19]1[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=1)[CH2:9][C:10]([C:12]1[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=1)=O)=O)[CH3:2].C([O-])(=O)C.[NH4+:31]>C(O)(=O)C>[CH2:1]([O:3][C:4](=[O:26])[CH2:5][C:6]1[N:8]([C:19]2[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=2)[CH:9]=[C:10]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[N:31]=1)[CH3:2]
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 517165Ammonium AcetateHCID 86687939N-(4-fluoro-phenyl)-N-(2-(4-fluoro-phenyl)-2-oxo-ethyl)-malonamic acid ethyl ester

生成物 1

HCID 86687938(1,4-bis-(4-fluoro-phenyl)-1H-imidazol-2-yl)-acetic acid ethyl ester収率 8.8%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

1.2 g N-(4-fluoro-phenyl)-N-(2-(4-fluoro-phenyl)-2-oxo-ethyl)-malonamic acid ethyl ester and 1.8 g ammonium acetate in 20 mL concentrated acetic acid were refluxed 4 h. The reaction was evaporated. Water was added to the residue and the mixture was extracted with DCM. The organic layer was dried and evaporated. The residue was purified by chromatography on silica (100% dichlormethane) to yield 100 mg of the desired compound. Rt: 1.39 min (method B), (M+H)+: 343

後処理

  1. customThe reaction was evaporated
  2. additionWater was added to the residue
  3. extractionthe mixture was extracted with DCM
  4. customThe organic layer was dried
  5. customevaporated
  6. customThe residue was purified by chromatography on silica (100% dichlormethane)

出典と根拠

ORDレコード
ord-56941b4d3859417e8a31a7741b6efb46
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08937176B2

反応ノート

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