O-Phenylenediamine → 2-(5-Methylpyridin-2-yl)benzimidazole

HRID 1449020

反応式

HRID 1449020 の反応式
[C:1]1([NH2:8])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH2:7].[CH3:9][C:10]1[CH:11]=[CH:12][C:13]([C:16](O)=O)=[N:14][CH:15]=1.C(=O)([O-])[O-].[Na+].[Na+]>O>[CH3:9][C:10]1[CH:11]=[CH:12][C:13]([C:16]2[NH:7][C:2]3[CH:3]=[CH:4][CH:5]=[CH:6][C:1]=3[N:8]=2)=[N:14][CH:15]=1

参加物

5

反応物 3

HCID 7243O-PhenylenediamineHCID 10340Sodium CarbonateHCID 1995755-Methylpicolinic acid

生成物 1

HCID 203478002-(5-Methylpyridin-2-yl)benzimidazole

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

6.2 g. of o-phenylenediamine, 7.1 g. of 5-methylpicolinic acid and 40 g. of polyphosphoric acid were stirred under nitrogen gas current at 160° C. to 180° C. for 4 hours. To the reaction mixture were added 400 ml. of water and then a concentrated aqueous solution of sodium carbonate to neutrality. The resulting crystals were filtered off, dried and recrystallized from acetonitrile or ethyl acetate to obtain 9.4 g. of colorless needles of the product (86% of theory), M.P. 229.0°-229.5° C.

後処理

  1. additionTo the reaction mixture were added 400 ml
  2. filtrationThe resulting crystals were filtered off
  3. customdried
  4. customrecrystallized from acetonitrile or ethyl acetate
  5. customto obtain 9.4 g

出典と根拠

ORDレコード
ord-91f87d1198134f97a0820547c530d953
出典データセット
uspto-grants-1980_02
特許番号
US04188486

関連ノート

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