Methyl 6-fluoro-2-methyl-3-nitrobenzoate → Benzoic acid, 3-amino-6-fluoro-2-methyl-, methyl ester
反応式
[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]参加物
4
実験手順
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%).
後処理
- 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)
出典と根拠
- ORDレコード
- ord-ea6640d6148146818e7881acfd430e9a
- 出典データセット
- uspto-grants-2012_02
- 特許番号
- US08110585B2
反応ノート
読み込み中…