Imidazole → 4-ethoxycarbonyl-5-methyl-1-(2-nitro-5-(1-imidazolyl)phenyl)-1H-imidazole

HRID 1599430ノート

反応式

HRID 1599430 の反応式
[CH2:1]([O:3][C:4]([C:6]1[N:7]=[CH:8][N:9]([C:12]2[CH:17]=[C:16](F)[CH:15]=[CH:14][C:13]=2[N+:19]([O-:21])=[O:20])[C:10]=1[CH3:11])=[O:5])[CH3:2].[NH:22]1[CH:26]=[CH:25][N:24]=[CH:23]1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH2:1]([O:3][C:4]([C:6]1[N:7]=[CH:8][N:9]([C:12]2[CH:17]=[C:16]([N:22]3[CH:26]=[CH:25][N:24]=[CH:23]3)[CH:15]=[CH:14][C:13]=2[N+:19]([O-:21])=[O:20])[C:10]=1[CH3:11])=[O:5])[CH3:2]

参加物

5

反応物 3

HCID 795ImidazoleHCID 11430Potassium CarbonateHCID 189281094-ethoxycarbonyl-5-methyl-1-(2-nitro-5-fluorophenyl)-1H-imidazole

生成物 1

HCID 189281334-ethoxycarbonyl-5-methyl-1-(2-nitro-5-(1-imidazolyl)phenyl)-1H-imidazole収率 61%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
80 °C

実験手順

A mixture of 4-ethoxycarbonyl-5-methyl-1-(2-nitro-5-fluorophenyl)-1H-imidazole (20.0 g, 68 mmol), imidazole (4.7 g, 69 mmol), potassium carbonate (9.5 g, 69 mmol) and acetonitrile (150 ml) was stirred at 80° C. for 16 h. The solvent was removed under reduced pressure and the residue dissolved in ethyl acetate and washed twice with water. The organic phase was dried (MgSO4), filtered and evaporated in vacuo to give 14.1 g (61%) of 4-ethoxycarbonyl-5-methyl-1-(2-nitro-5-(1-imidazolyl) phenyl)-1H-imidazole.

後処理

  1. customThe solvent was removed under reduced pressure
  2. dissolutionthe residue dissolved in ethyl acetate
  3. washwashed twice with water
  4. dry with materialThe organic phase was dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-7d2148cafa414b69ad250edd81a981e0
出典データセット
uspto-grants-1998_04
特許番号
US05741785

反応ノート

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