3,5-Difluoropyridine-2-carboxylic acid → 3,5-difluoro-N-methylpyridine-2-carboxamide
반응식
[F:1][C:2]1[C:3]([C:9]([OH:11])=O)=[N:4][CH:5]=[C:6]([F:8])[CH:7]=1.[CH3:12][NH2:13].CO>C1COCC1>[F:1][C:2]1[C:3]([C:9]([NH:13][CH3:12])=[O:11])=[N:4][CH:5]=[C:6]([F:8])[CH:7]=1참가 물질
4
반응 조건
- 온도
- 50 °C
실험 절차
N,N′-carbonyldiimidazole (600 mg) was added to a solution of 3,5-difluoropyridine-2-carboxylic acid (500 mg) in THF (10 ml), followed by stirring at 50° C. for one hour. The reaction solution was returned to room temperature, a 40% methylamine/methanol solution (1 ml) was added thereto, followed by stirring at room temperature for one hour. The reaction solution was concentrated and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0 to 0:100 linear gradient) to obtain 3,5-difluoro-N-methylpyridine-2-carboxamide (293 mg) as a colorless solid.
후처리
- customwas returned to room temperature
- stirringby stirring at room temperature for one hour
- concentrationThe reaction solution was concentrated
- customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0 to 0:100 linear gradient)
출처 및 근거
- ORD 기록
- ord-542ff3a5fff6400e99c84b91f9847ebe
- 출처 데이터셋
- uspto-grants-2013_02
- 특허 번호
- US08377923B2
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