反応式
[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([O:11][CH3:12])[C:3]=1[C:4]([OH:6])=O.[CH3:13][O:14][C:15]1[CH:43]=[CH:42][C:18]([CH2:19][N:20]2[CH:24]=[C:23]([NH2:25])[C:22]([C:26]3[NH:30][C:29]4[CH:31]=[CH:32][C:33]([CH2:35][N:36]5[CH2:41][CH2:40][O:39][CH2:38][CH2:37]5)=[CH:34][C:28]=4[N:27]=3)=[N:21]2)=[CH:17][CH:16]=1.C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1>CN(C=O)C>[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([O:11][CH3:12])[C:3]=1[C:4]([NH:25][C:23]1[C:22]([C:26]2[NH:30][C:29]3[CH:31]=[CH:32][C:33]([CH2:35][N:36]4[CH2:37][CH2:38][O:39][CH2:40][CH2:41]4)=[CH:34][C:28]=3[N:27]=2)=[N:21][N:20]([CH2:19][C:18]2[CH:42]=[CH:43][C:15]([O:14][CH3:13])=[CH:16][CH:17]=2)[CH:24]=1)=[O:6]参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
A mixture of 2-fluoro-6-methoxy-benzoic acid (20 mg, 0.12 mmol), 1-(4-methoxy-benzyl)-3-(5-morpholin-4-ylmethyl-1H-benzimidazol-2-yl)-1H-pyrazol-4-ylamine (50 mg, 0.12 mmol), EDC (116 mg, 0.14 mmol) and HOBt (81 mg, 0.14 mmol) was stirred at room temperature in DMF (2 ml) for 20 h. The mixture was reduced in vacuo and the residue partitioned between EtOAc (5 ml) and water (2 ml) and the organic portion washed with saturated aqueous sodium hydrogen carbonate, dried (MgSO4) and reduced in vacuo. The residue was purified by flash column chromatography [SiO2, EtOAc] to give 2-fluoro-6-methoxy-N-[1-(4-methoxy-benzyl)-3-(5-morpholin-4-ylmethyl-1H-benzimidazol-2-yl)-1H-pyrazol-4-yl]-benzamide as a white solid (80 mg, 61%).
後処理
- customthe residue partitioned between EtOAc (5 ml) and water (2 ml)
- washthe organic portion washed with saturated aqueous sodium hydrogen carbonate
- dry with materialdried (MgSO4)
- customThe residue was purified by flash column chromatography [SiO2, EtOAc]
出典と根拠
- ORDレコード
- ord-58982af27e744215af82f12c374b6a66
- 出典データセット
- uspto-grants-2011_07
- 特許番号
- US07977477B2
関連ノート
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