N-bromobutanimide → Methyl 3-amino-6-bromo-5-fluoro-2-methylbenzoate
反応式
[NH2:1][C:2]1[C:3]([CH3:13])=[C:4]([CH:9]=[C:10]([F:12])[CH:11]=1)[C:5]([O:7][CH3:8])=[O:6].[Br:14]N1C(=O)CCC1=O>C(#N)C>[NH2:1][C:2]1[C:3]([CH3:13])=[C:4]([C:9]([Br:14])=[C:10]([F:12])[CH:11]=1)[C:5]([O:7][CH3:8])=[O:6]参加物
4
実験手順
To a solution of methyl 3-amino-5-fluoro-2-methylbenzoate (1.37 g, 7.48 mmol) in acetonitrile (57 mL) was added N-bromosuccinimide (1.01 g, 5.66 mmol) under ice-cooling, and the mixture was stirred for 2 hr. The reaction solution was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/hexane=10/90→30/70) to give the title compound (1.33 g, yield 68%).
後処理
- temperaturecooling
- concentrationThe reaction solution was concentrated under reduced pressure
- customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane=10/90→30/70)
出典と根拠
- ORDレコード
- ord-dcc2122e14cb48eb99102b147426f582
- 出典データセット
- uspto-grants-2012_08
- 特許番号
- US08247429B2
反応ノート
読み込み中…