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

HRID 16134

反応式

HRID 16134 の反応式
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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
90 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-45a00e9379fe4e9aa2e1505c54eed664
出典データセット
uspto-grants-2010_06
特許番号
US07737143B2

関連ノート

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