反応 #57145

反応方程式

[3-(4-{[(phenylamino)carbonyl]amino}phenyl)-4-(1H-pyrrolo[2,3-b]pyridin-4-yl)-1H-pyrazol-1-yl]acetic acid

1-ethyl-3-(3-dimethylaminopropyl)carbodiimide

m-anisidine

→

title compound

収率 26.0%

N-[3-(methyloxy)phenyl]-2-[3-(4-{[(phenylamino)carbonyl]amino}phenyl)-4-(1H-pyrrolo[2,3-b]pyridin-4-yl)-1H-pyrazol-1-yl]acetamide

収率 26.0%

溶媒

N,N-dimethylformamide

反応条件

後処理

1. 1
   濃縮concentrated in vacuo
2. 2
   洗浄washed with saturated aqueous sodium bicarbonate (10 mL)
3. 3
   乾燥The organic layer was dried over sodium sulfate
4. 4
   濃縮concentrated in vacuo
5. 5
   その他Purification by Gilson reverse phase HPLC

実験手順

To a solution of [3-(4-{[(phenylamino)carbonyl]amino}phenyl)-4-(1H-pyrrolo[2,3-b]pyridin-4-yl)-1H-pyrazol-1-yl]acetic acid (0.166 mmol), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (0.249 mmol), 4-dimethylaminopyridine (0.249 mmol) and N,N-dimethylformamide (3.2 mL) at room temperature was added m-anisidine (0.415 mmol). The reaction mixture was stirred overnight at room temperature, concentrated in vacuo, taken up in ethyl acetate (10 mL) and washed with saturated aqueous sodium bicarbonate (10 mL). The organic layer was dried over sodium sulfate and concentrated in vacuo. Purification by Gilson reverse phase HPLC afforded the title compound as a white solid (26%). ESMS [M+H]+: 558.4

出典