Nitric Acid → 2-Hydroxy-3-methyl-5-nitro-benzonitrile
反応式
[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH3:9])[C:4]=1[OH:10])#[N:2].[N+:11]([O-])([OH:13])=[O:12].O>C(O)(=O)C>[C:1]([C:3]1[CH:8]=[C:7]([N+:11]([O-:13])=[O:12])[CH:6]=[C:5]([CH3:9])[C:4]=1[OH:10])#[N:2]参加物
5
反応条件
- 温度
- 45 °C
実験手順
To a heated (45° C.), stirred solution of 2-cyano-6-methylphenol (5 g) in glacial acetic acid (32 mL) was added a solution of fuming nitric acid (3.2 mL) in acetic acid (12 mL). After 1 h at elevated temperature (45° C.), the reaction mixture was cooled (to 0° C.), water added and partitioned between DEE/water. The organic phase was washed with water, brine, dried over sodium sulfate and concentrated in vacuo to afford a solid. Recrystallization from DEE afforded the title compound as yellow crystals (3.6 g).
後処理
- additionadded
- custompartitioned between DEE/water
- washThe organic phase was washed with water, brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated in vacuo
- customto afford a solid
- customRecrystallization from DEE
出典と根拠
- ORDレコード
- ord-418ea8f2777c4d5c9453a9cc0359d90b
- 出典データセット
- uspto-grants-2001_02
- 特許番号
- US06194454B1
反応ノート
読み込み中…