반응식
[H-].[Na+].[F:3][C:4]([F:18])([F:17])[C:5]1[CH:10]=[CH:9][N:8]=[C:7]([C:11]2[NH:12][O:13][C:14](=[O:16])[N:15]=2)[CH:6]=1.[F:19][C:20]1[CH:30]=[CH:29][C:23]([C:24]([O:26][CH2:27]Cl)=[O:25])=[CH:22][CH:21]=1.[Cl-].[NH4+]>CN(C)C=O>[F:19][C:20]1[CH:21]=[CH:22][C:23]([C:24]([O:26][CH2:27][N:15]2[C:14](=[O:16])[O:13][N:12]=[C:11]2[C:7]2[CH:6]=[C:5]([C:4]([F:3])([F:17])[F:18])[CH:10]=[CH:9][N:8]=2)=[O:25])=[CH:29][CH:30]=1참가 물질
실험 절차
Into 2 ml of N,N-dimethylformamide was suspended 0.07 g of sodium hydride (60% oily), and 0.3 g of 3-(4-trifluoromethylpyridin-2-yl)-1,2,4-oxadiazol-5-one was added at room temperature. After stirring for 15 minutes, 0.29 g of chloromethyl 4-fluorobenzoate was added, and the mixture was stirred at 70° C. for 4 hours. The reaction solution was allowed to cool to room temperature, and poured into an aqueous saturated ammonium chloride solution, followed by extraction with ethyl acetate three times. The organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.17 g of [3-(4-trifluoromethylpyridin-2-yl)-1,2,4-oxadiazol-5-on-4-yl]methyl 4-fluorobenzoate (present compound (38)).
후처리
- additionwas added at room temperature
- stirringthe mixture was stirred at 70° C. for 4 hours
- extractionfollowed by extraction with ethyl acetate three times
- washwashed with an aqueous saturated sodium chloride solution
- dry with materialdried with anhydrous magnesium sulfate
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-2ae16a5139b847cba2266c2b81f198a7
- 출처 데이터셋
- uspto-grants-2012_11
- 특허 번호
- US08318776B2
연결된 노트
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