Nitric Acid → 2-Hydroxy-3-methyl-5-nitro-benzonitrile
반응식
[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]참가 물질
5
반응 조건
- 온도
- 45 °C
실험 절차
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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-418ea8f2777c4d5c9453a9cc0359d90b
- 출처 데이터셋
- uspto-grants-2001_02
- 특허 번호
- US06194454B1
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