Pyrazole → HCID 68485174、化合物

HRID 383289ノート

反応式

HRID 383289 の反応式
Cl[C:2]1[CH:7]=[C:6]([C:8]2[N:12]3[CH:13]=[C:14]([NH:17][CH:18]4[CH2:23][CH2:22][CH:21]([OH:24])[CH2:20][CH2:19]4)[CH:15]=[CH:16][C:11]3=[N:10][CH:9]=2)[CH:5]=[CH:4][N:3]=1.[NH:25]1[CH:29]=[CH:28][CH:27]=[N:26]1.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C=O)C>[N:25]1([C:2]2[CH:7]=[C:6]([C:8]3[N:12]4[CH:13]=[C:14]([NH:17][CH:18]5[CH2:23][CH2:22][CH:21]([OH:24])[CH2:20][CH2:19]5)[CH:15]=[CH:16][C:11]4=[N:10][CH:9]=3)[CH:5]=[CH:4][N:3]=2)[CH:29]=[CH:28][CH:27]=[N:26]1

参加物

5

反応物 3

HCID 1048PyrazoleHCID 10796Cesium carbonateHCID 252619024-[3-(2-Chloro-pyridin-4-yl)-imidazo[1,2-a]pyridin-6-ylamino]-cyclohexanol

生成物 1

HCID 68485174HCID 68485174、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture comprising [4-[3-(2-Chloro-pyridin-4-yl)-imidazo[1,2-a]pyridin-6-ylamino]-cyclohexanol (Example 2.1) (1 eq, 0.29 mmol, 100 mg), pyrazole (5 eq, 1.45 mmol, 99 mg) and cesium carbonate (3 eq, 0.87 mmol, 284 mg) in DMF (25 ml) is heated using microwave radiation at 145° C. for 6 hours. After cooling to room temperature, the mixture is loaded onto a SCX-2 cartridge eluting with MeOH followed by 2M NH3 in MeOH. The solvent is removed in vacuo and the crude product is triturated with ethyl acetate to afford the title compound; [M+H]+=375

後処理

  1. temperatureis heated
  2. customat 145° C.
  3. customfor 6 hours
  4. washeluting with MeOH
  5. customThe solvent is removed in vacuo
  6. customthe crude product is triturated with ethyl acetate

出典と根拠

ORDレコード
ord-06cc73b89da14582ab5ac35f6b642553
出典データセット
uspto-grants-2013_02
特許番号
US08367662B2

反応ノート

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