Cesium carbonate → 1-(6-chloropyrazin-2-yl)-1H-benzimidazole-6-carboxamide

HRID 16134

반응식

HRID 16134 반응식
Cl[C:2]1[CH:7]=[N:6][CH:5]=[C:4]([Cl:8])[N:3]=1.[NH:9]1[C:13]2[CH:14]=[CH:15][C:16]([C:18]([NH2:20])=[O:19])=[CH:17][C:12]=2[N:11]=[CH:10]1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C=O)C.C(OCC)(=O)C>[Cl:8][C:4]1[N:3]=[C:2]([N:11]2[C:12]3[CH:17]=[C:16]([C:18]([NH2:20])=[O:19])[CH:15]=[CH:14][C:13]=3[N:9]=[CH:10]2)[CH:7]=[N:6][CH:5]=1

참가 물질

6

반응물 3

HCID 10796Cesium carbonateHCID 785042,6-DichloropyrazineHCID 154216421H-Benzimidazole-6-carboxamide

생성물 1

HCID 588699191-(6-chloropyrazin-2-yl)-1H-benzimidazole-6-carboxamide

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
90 °C

실험 절차

A mixture of 2,6-dichloropyrazine (2.0 g, 13.4 mmol), 1H-benzimidazole-5-carboxamide (2.0 g, 12.3 mmol) and cesium carbonate (5.6 g, 17.2 mmol) in DMF (10 mL) was heated at 90° C. for 3 h. The solution was cooled to RT and diluted with ethyl acetate (20 mL) and filtered. The solid material was washed with chloroform-methanol (20 mL, 4:1) and the combined filtrates concentrated in vacuo. The residue thus obtained (3.02 g) was used without further purification.

후처리

  1. temperatureThe solution was cooled to RT
  2. filtrationfiltered
  3. washThe solid material was washed with chloroform-methanol (20 mL, 4:1)
  4. concentrationthe combined filtrates concentrated in vacuo
  5. customThe residue thus obtained (3.02 g)
  6. customwas used without further purification

출처 및 근거

ORD 기록
ord-45a00e9379fe4e9aa2e1505c54eed664
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737143B2

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