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Pyridine → HCID 178430970, 화합물

HRID 968794
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HRID 968794 반응식
[CH3:1][C:2]1[C:7]2[NH:8][CH:9]=[N:10][C:6]=2[C:5]([C:11](O)=[O:12])=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15].S(N)([NH2:20])(=O)=O.N1C=CC=CC=1>O>[CH3:1][C:2]1[C:7]2[NH:8][CH:9]=[N:10][C:6]=2[C:5]([C:11]([NH2:20])=[O:12])=[CH:4][C:3]=1[N+:14]([O-:16])=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 82267SulfamideHCID 178430971HCID 178430971, 화합물

생성물 1

HCID 178430970HCID 178430970, 화합물수율 85.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 7-Methyl-6-nitro-1H-benzimidazole-4-carboxylic Acid (23) (0.692 g, 3.12 mmol), sulfamide (0.600 g, 6.26 mmol), and pyridine (8 mL) is heated at reflux for about 16 hours. The resulting heterogeneous reaction mixture is cooled to ambient temperature, diluted with water (10 mL) and cooled to 0° C. for 1 hour. The solids that form are filtered, washed with water (10 mL) and methanol (10 mL), and dried to obtain 7-Methyl-6-nitro-1H-benzimidazole-4-carboxamide (25) as a cream colored solid (0.586 g, 85% yield).

후처리

  1. temperatureis heated
  2. temperatureat reflux for about 16 hours
  3. temperaturecooled to 0° C. for 1 hour
  4. filtrationThe solids that form are filtered
  5. washwashed with water (10 mL) and methanol (10 mL)
  6. customdried

출처 및 근거

ORD 기록
ord-133e330d35fb4bce9aa6ed0269430265
출처 데이터셋
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07304084B2

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