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Water → 1-Ethyl-3-{5-[(3-methyl-3H-imidazo[4,5-b]pyridin-2-yl)oxy]pyridin-2-yl}-1H-pyrazolo[4,3-b]pyridine

HRID 573326
ノート
印刷プレビュー

反応式

HRID 573326 の反応式
[CH3:1][N:2]1[C:6]2=[N:7][CH:8]=[CH:9][CH:10]=[C:5]2[N:4]=[C:3]1S(C)(=O)=O.[CH2:15]([N:17]1[C:25]2[C:20](=[N:21][CH:22]=[CH:23][CH:24]=2)[C:19]([C:26]2[N:31]=[CH:30][C:29]([OH:32])=[CH:28][CH:27]=2)=[N:18]1)[CH3:16].[H-].[Na+].O>CN(C=O)C>[CH2:15]([N:17]1[C:25]2[C:20](=[N:21][CH:22]=[CH:23][CH:24]=2)[C:19]([C:26]2[CH:27]=[CH:28][C:29]([O:32][C:3]3[N:2]([CH3:1])[C:6]4=[N:7][CH:8]=[CH:9][CH:10]=[C:5]4[N:4]=3)=[CH:30][N:31]=2)=[N:18]1)[CH3:16]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 585773713-Methyl-2-(methylsulfonyl)-3H-imidazo[4,5-b]pyridineHCID 1363976906-(1-Ethyl-1H-pyrazolo[4,3-b]pyridin-3-yl)pyridin-3-ol

生成物 1

HCID 667281201-Ethyl-3-{5-[(3-methyl-3H-imidazo[4,5-b]pyridin-2-yl)oxy]pyridin-2-yl}-1H-pyrazolo[4,3-b]pyridine収率 36.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

To a mixture of 3-methyl-2-(methylsulfonyl)-3H-imidazo[4,5-b]pyridine (90 mg) and 6-(1-ethyl-1H-pyrazolo[4,3-b]pyridin-3-yl)pyridin-3-ol (68 mg) in DMF (1 mL) was added NaH (60% in oil, 18.11 mg), and the mixture was stirred at 100° C. for 1 h. The mixture was heated at 180° C. for 30 min under microwave irradiation. The mixture was poured into water and extracted with AcOEt. The organic layer was separated, washed with brine, dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (AcOEt/hexane). The eluent was evaporated and the residue was crystallized from EtOH/hexane to give the title compound (38.1 mg).

後処理

  1. temperatureThe mixture was heated at 180° C. for 30 min under microwave irradiation
  2. extractionextracted with AcOEt
  3. customThe organic layer was separated
  4. washwashed with brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by basic silica gel column chromatography (AcOEt/hexane)
  8. customThe eluent was evaporated
  9. customthe residue was crystallized from EtOH/hexane

出典と根拠

ORDレコード
ord-af457ea6be4b47148d654058b1651c55
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09029536B2

反応ノート

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