반응식
[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]참가 물질
5
반응 조건
- 온도
- 50 °C
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-b5c50467b3414a24b1e17740877d3a23
- 출처 데이터셋
- uspto-grants-2013_12
- 특허 번호
- US08609705B2
연결된 노트
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