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

HRID 1449020

반응식

HRID 1449020 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-91f87d1198134f97a0820547c530d953
출처 데이터셋
uspto-grants-1980_02
특허 번호
US04188486

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