Nitric Acid → 6-Fluoro-2-methyl-3-nitrobenzoic acid
反応式
[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([CH3:11])[C:3]=1[C:4]([OH:6])=[O:5].[N+:12]([O-])([OH:14])=[O:13]>S(=O)(=O)(O)O>[F:1][C:2]1[C:3]([C:4]([OH:6])=[O:5])=[C:7]([CH3:11])[C:8]([N+:12]([O-:14])=[O:13])=[CH:9][CH:10]=1参加物
4
反応条件
- 温度
- -15 °C
実験手順
2-Fluoro-6-methylbenzoic acid (40 g, 0.26 mol) was dissolved in 320 mL of sulfuric acid and chilled to −15° C. To this was added 14 mL of fuming nitric acid in 60 mL of sulfuric acid over a 10 minute period. Once the addition was complete, the mixture was stirred at 0° C. for 1 hour, then poured into ice water, and stirred. The resulting solids were collected and then dissolved in EtOAc, which was washed with water, dried over sodium sulfate and concentrated to 50 g (97%) of the title compound.
後処理
- additionOnce the addition
- stirringstirred
- customThe resulting solids were collected
- dissolutiondissolved in EtOAc
- washwhich was washed with water
- dry with materialdried over sodium sulfate
- concentrationconcentrated to 50 g (97%) of the title compound
出典と根拠
- ORDレコード
- ord-f1c2ceebcd89488ea38b1e329df9b862
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09174981B2
反応ノート
読み込み中…