Cesium carbonate → 1-neopentyl-4-(4-nitrophenyl)-1H-imidazole

HRID 873589ノート

反応式

HRID 873589 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]2[N:11]=[CH:12][NH:13][CH:14]=2)=[CH:6][CH:5]=1)([O-:3])=[O:2].C(=O)([O-])[O-].[Cs+].[Cs+].Br[CH2:22][C:23]([CH3:26])([CH3:25])[CH3:24]>CN(C)C=O.C(OCC)(=O)C>[CH2:22]([N:13]1[CH:14]=[C:10]([C:7]2[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:9][CH:8]=2)[N:11]=[CH:12]1)[C:23]([CH3:26])([CH3:25])[CH3:24]

参加物

6

反応物 3

HCID 10796Cesium carbonateHCID 124151-Bromo-2,2-dimethylpropaneHCID 178418805HCID 178418805、化合物

生成物 1

HCID 867020761-neopentyl-4-(4-nitrophenyl)-1H-imidazole

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 4-(4-nitrophenyl)-1H-imidazole (0.500 g, 2.64 mmol) in N,N-dimethylformamide (10 ml) was added cesium carbonate (1.292 g, 3.96 mmol) followed by 1-bromo-2,2-dimethylpropane (0.366 ml, 2.91 mmol). After heating at 85° overnight, the reaction mixture was cooled to room temperature, diluted with ethyl acetate, washed with water and brine, dried over magnesium sulfate, filtered and concentrated. Normal phase chromatography provided the title compound.

後処理

  1. temperatureAfter heating at 85° overnight
  2. washwashed with water and brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-4a67a282fd81477783e1d0d70467bbff
出典データセット
uspto-grants-2015_03
特許番号
US08975398B2

反応ノート

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