反応式
[N:1]1[CH:2]=[C:3]([C:10]([OH:12])=O)[N:4]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=12.ClC1C=C(Cl)C=C(Cl)C=1C(Cl)=O.C(N(CC)CC)C.[CH2:32]([C:34]1[C:42]2[C:41]([NH2:43])=[CH:40][CH:39]=[CH:38][C:37]=2[N:36]([CH2:44][C:45]2[CH:49]=[CH:48][N:47]([CH3:50])[N:46]=2)[N:35]=1)[CH3:33]>CN1C(=O)CCC1.[OH-].[Na+].CCOC(C)=O>[CH2:32]([C:34]1[C:42]2[C:37](=[CH:38][CH:39]=[CH:40][C:41]=2[NH:43][C:10]([C:3]2[N:4]3[CH:9]=[CH:8][CH:7]=[CH:6][C:5]3=[N:1][CH:2]=2)=[O:12])[N:36]([CH2:44][C:45]2[CH:49]=[CH:48][N:47]([CH3:50])[N:46]=2)[N:35]=1)[CH3:33]参加物
8
反応物 4
生成物 1
試薬・触媒・溶媒 3
反応条件
- 温度
- 87 °C
実験手順
To a suspension of imidazo[1,2-a]pyridine-3-carboxylic acid (47.6 mg, 0.294 mmol) in NMP (4 mL) was added 2,4,6-trichlorobenzoyl chloride (45.9 μL, 0.294 mmol) and triethylamine (40.9 μL, 0.294 mmol). The reaction mixture was stirred for 30 minutes. 3-Ethyl-1-((1-methyl-1H-pyrazol-3-yl)methyl)-1H-indazol-4-amine (50 mg, 0.196 mmol) was added and the mixture was heated at 87° C. for three hours. The mixture was cooled to ambient temperature and diluted with 10% NaOH aqueous solution (5 mL) and EtOAc (20 mL). The organic phase was washed with water and brine and concentrated under reduced pressure. The residue was triturated with Et2O to give the final product (52 mg). MS (ES+APCI) m/z=400 (M+H).
後処理
- temperatureThe mixture was cooled to ambient temperature
- washThe organic phase was washed with water and brine
- concentrationconcentrated under reduced pressure
- customThe residue was triturated with Et2O
出典と根拠
- ORDレコード
- ord-0760290c1a674d74bca94200b7cbeb2b
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08841455B2
関連ノート
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