反応式
[I:1][C:2]1[CH:10]=[N:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=O.CCN=C=NCCCN(C)C.[NH2:22][C:23]1[CH:28]=[C:27]([C:29]([F:32])([F:31])[F:30])[CH:26]=[CH:25][C:24]=1[OH:33]>N1C=CC=CC=1>[OH:33][C:24]1[CH:25]=[CH:26][C:27]([C:29]([F:30])([F:31])[F:32])=[CH:28][C:23]=1[NH:22][C:4](=[O:6])[C:3]1[CH:7]=[CH:8][N:9]=[CH:10][C:2]=1[I:1]参加物
5
反応条件
- 温度
- 50 °C
実験手順
A mixture of 1.78 g of 3-iodo-isonicotinic acid, 1.38 g of WSC and 12 ml of pyridine was stirred while heating at 50° C. for 15 minutes. Then, 1.15 g of 2-amino-4-(trifluoromethyl)phenol was added to the reaction mixture. The reaction mixture was stirred while heating at 80° C. for two hours. The reaction mixture was returned to room temperature, and concentrated under reduced pressure. Water was added to the residue, followed by extraction with ethyl acetate. The organic layer was washed with a saturated sodium chloride solution, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure to give 1.81 g of N-[2-hydroxy-5-(trifluoromethyl)phenyl]-3iodo isonicotinamide.
後処理
- stirringThe reaction mixture was stirred
- temperaturewhile heating at 80° C. for two hours
- customwas returned to room temperature
- concentrationconcentrated under reduced pressure
- additionWater was added to the residue
- extractionfollowed by extraction with ethyl acetate
- washThe organic layer was washed with a saturated sodium chloride solution
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-b5c50467b3414a24b1e17740877d3a23
- 出典データセット
- uspto-grants-2013_12
- 特許番号
- US08609705B2
関連ノート
読み込み中…