Ethanol → 3-[5-(2-Amino-pyrimidin-5-yl)-1-tert-butyl-1H-benzimidazol-2-yl]-4-1,2,4-triazol-1-yl-benzoic acid

HRID 1966746ノート

反応式

HRID 1966746 の反応式
[NH2:1][C:2]1[N:7]=[CH:6][C:5]([C:8]2[CH:33]=[CH:32][C:11]3[N:12]([C:28]([CH3:31])([CH3:30])[CH3:29])[C:13]([C:15]4[CH:16]=C([CH:20]=[CH:21][C:22]=4[N:23]4[CH:27]=[N:26][CH:25]=[N:24]4)C#N)=[N:14][C:10]=3[CH:9]=2)=[CH:4][N:3]=1.[OH-:34].[K+].[CH3:36][CH2:37][OH:38]>O>[NH2:1][C:2]1[N:7]=[CH:6][C:5]([C:8]2[CH:33]=[CH:32][C:11]3[N:12]([C:28]([CH3:31])([CH3:30])[CH3:29])[C:13]([C:15]4[CH:16]=[C:36]([CH:20]=[CH:21][C:22]=4[N:23]4[CH:27]=[N:26][CH:25]=[N:24]4)[C:37]([OH:34])=[O:38])=[N:14][C:10]=3[CH:9]=2)=[CH:4][N:3]=1

参加物

5

反応物 3

HCID 702EthanolHCID 14797Potassium HydroxideHCID 532376053-[5-(2-Amino-pyrimidin-5-yl)-1-tert-butyl-1H-benzimidazol-2-yl]-4-1,2,4-triazol-1-yl-benzonitrile

生成物 1

HCID 585419673-[5-(2-Amino-pyrimidin-5-yl)-1-tert-butyl-1H-benzimidazol-2-yl]-4-1,2,4-triazol-1-yl-benzoic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

To a mixture of 3-[5-(2-amino-pyrimidin-5-yl)-1-tert-butyl-1H-benzimidazol-2-yl]-4-1,2,4-triazol-1-yl-benzonitrile (Example 7) (400 mg, 0.92 mmol) in EtOH (10 mL) is added KOH (103 mg, 1.8 mmol) in H2O (1 mL) at room temperature. The mixture is heated to 80° C. for 48 hours. The solution is cooled down and is concentrated under vacuum. The residue is dissolved in H2O (10 mL) and the pH of the solution is adjusted to 6 with 2M HCl solution. The white solid that precipitates out from the solution is collected by filtration. The white solid is dried under vacuum providing the title compound. LCMS (ESMS): m/z 455.20 (M++1)

後処理

  1. temperatureThe solution is cooled down
  2. concentrationis concentrated under vacuum
  3. dissolutionThe residue is dissolved in H2O (10 mL)
  4. customThe white solid that precipitates out from the solution
  5. filtrationis collected by filtration
  6. customThe white solid is dried under vacuum

出典と根拠

ORDレコード
ord-354e54afbd2d4a1c9f4d849a813b6673
出典データセット
uspto-grants-2013_04
特許番号
US08420655B2

反応ノート

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