Methyl 6-fluoro-2-methyl-3-nitrobenzoate → Benzoic acid, 3-amino-6-fluoro-2-methyl-, methyl ester
반응식
[F:1][C:2]1[C:7]([C:8]([O:10][CH3:11])=[O:9])=[C:6]([CH3:12])[C:5]([N+:13]([O-])=O)=[CH:4][CH:3]=1>CO.[C].[Pd]>[NH2:13][C:5]1[C:6]([CH3:12])=[C:7]([C:2]([F:1])=[CH:3][CH:4]=1)[C:8]([O:10][CH3:11])=[O:9]참가 물질
4
실험 절차
To a solution of a crudely purified product (27.7 g, 130 mmol) of methyl 6-fluoro-2-methyl-3-nitrobenzoate in methanol (260 mL) was added palladium carbon (6.00 g, 10 wt %) and the mixture was stirred under hydrogen atmosphere for 12 hr. The catalyst was filtered off through celite, the filtrate was concentrated under reduced pressure, and the residue was purified by flash silica gel column chromatography (ethyl acetate/hexane=1/1) to give the title compound (15.0 g, yield 63%).
후처리
- filtrationThe catalyst was filtered off through celite
- concentrationthe filtrate was concentrated under reduced pressure
- customthe residue was purified by flash silica gel column chromatography (ethyl acetate/hexane=1/1)
출처 및 근거
- ORD 기록
- ord-ea6640d6148146818e7881acfd430e9a
- 출처 데이터셋
- uspto-grants-2012_02
- 특허 번호
- US08110585B2
반응 노트
불러오는 중…