反応式
[NH2:1][C:2]1[N:7]=[CH:6][C:5]([O:8][C:9]2[CH:10]=[C:11]([NH:15][C:16]([C:18]3[CH:23]=[CH:22][CH:21]=[C:20](C)[N:19]=3)=[O:17])[CH:12]=[CH:13][CH:14]=2)=[CH:4][CH:3]=1.[C:25]1([CH3:35])[CH:30]=[CH:29][C:28]([S:31](Cl)(=[O:33])=[O:32])=[CH:27][CH:26]=1.N1C=CC=C[CH:37]=1>>[CH3:37][C:23]1[C:18]([C:16]([NH:15][C:11]2[CH:12]=[CH:13][CH:14]=[C:9]([O:8][C:5]3[CH:6]=[N:7][C:2]([NH:1][S:31]([C:28]4[CH:29]=[CH:30][C:25]([CH3:35])=[CH:26][CH:27]=4)(=[O:33])=[O:32])=[CH:3][CH:4]=3)[CH:10]=2)=[O:17])=[N:19][CH:20]=[CH:21][CH:22]=1参加物
4
反応条件
- 温度
- 80 °C
実験手順
A mixture of N-{3-[(6-aminopyridin-3-yl)oxy]phenyl}-6-methylpyridine-2-carboxamide (8.25 g, 25.8 mmol), p-toluenesulfonyl chloride (5.41 g, 28.4 mmol) and pyridine (50 mL) was stirred at 80° C. for 2 hr. The reaction solution was concentrated under reduced pressure, and ethyl acetate was added to the residue. The mixture was washed with aqueous sodium hydrogen carbonate solution, water and saturated brine, dried over anhydrous magnesium sulfate and filtrated. The filtrate was concentrated under reduced pressure, and the residue was washed with ethyl acetate-hexane to give the title compound (12.1 g, 99%) as a pale-brown solid.
後処理
- concentrationThe reaction solution was concentrated under reduced pressure, and ethyl acetate
- additionwas added to the residue
- washThe mixture was washed with aqueous sodium hydrogen carbonate solution, water and saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltrated
- concentrationThe filtrate was concentrated under reduced pressure
- washthe residue was washed with ethyl acetate-hexane
出典と根拠
- ORDレコード
- ord-edc7c2f83e504d17ae0b988c5ac5dc24
- 出典データセット
- uspto-grants-2012_11
- 特許番号
- US08304557B2
関連ノート
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