Nitric Acid → Methyl 2,6-Difluoro-3-nitrobenzoate
反応式
[N+:1]([O-:4])(O)=[O:2].[F:5][C:6]1[CH:15]=[CH:14][CH:13]=[C:12]([F:16])[C:7]=1[C:8]([O:10][CH3:11])=[O:9]>S(=O)(=O)(O)O>[F:5][C:6]1[C:15]([N+:1]([O-:4])=[O:2])=[CH:14][CH:13]=[C:12]([F:16])[C:7]=1[C:8]([O:10][CH3:11])=[O:9]参加物
4
反応条件
- 温度
- 0 °C
実験手順
Fuming nitric acid (11 g, 174 mmol) was added to a solution of methyl 2,6-difluorobenzoate (25 g, 145 mmol) in concentrated sulfuric acid (50 mL) at 0° C., and the reaction was stirred for 30 min at 0° C. The reaction mixture was poured over ice-water. The precipitate was filtered off by suction to give the desired product of Step B (25.1 g, 80.6%). 1H NMR (400 MHz, CDCl3) δ ppm 8.13-8.20 (m, 1H), 7.02-7.10 (m, 1H), 3.93 (s, 3H).
後処理
- filtrationThe precipitate was filtered off by suction
出典と根拠
- ORDレコード
- ord-7afa254142ab492989234cddc18c094f
- 出典データセット
- uspto-grants-2013_04
- 特許番号
- US08415345B2
反応ノート
読み込み中…