Nitric Acid → 3,5-Difluoro-4-nitrophenol
反応式
[F:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[C:6]([F:8])[CH:7]=1.[N+:10]([O-])([OH:12])=[O:11]>C(Cl)Cl>[F:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[C:6]([F:8])[C:7]=1[N+:10]([O-:12])=[O:11]参加物
4
実験手順
To a solution of 3,5-difluorophenol (10 g, 76.9 mmol) in CH2Cl2 at 0° Celsius was added 4.9 mL of 70% nitric acid dropwise. After addition was complete, the reaction was allowed to warm to room temperature and stirred for 1 hour. The reaction was poured into a separatory funnel and washed once with 750 mL water. The organic layer was dried with Na2SO4, filtered and concentrated to dryness. The resulting residue was purified via FCC to afford the title compound. 1H NMR (400 MHz, DMSO-d6) δ 6.81-6.67 (m, 2H), 3.40 (bs, 1H).
後処理
- additionAfter addition
- additionThe reaction was poured into a separatory funnel
- washwashed once with 750 mL water
- dry with materialThe organic layer was dried with Na2SO4
- filtrationfiltered
- concentrationconcentrated to dryness
- customThe resulting residue was purified via FCC
出典と根拠
- ORDレコード
- ord-681475cfcc954e0990353d08829e6661
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09089569B2
反応ノート
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