Nitric Acid → 1-Bromo-4-fluoro-2-methyl-5-nitrobenzene
反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[CH3:9].[N+:10]([O-])([OH:12])=[O:11]>S(=O)(=O)(O)O>[Br:1][C:2]1[CH:7]=[C:6]([N+:10]([O-:12])=[O:11])[C:5]([F:8])=[CH:4][C:3]=1[CH3:9]参加物
4
実験手順
Combine 1-bromo-4-fluoro-2-methylbenzene (30.0 g, 159 mmol) in concentrated sulfuric acid (100 mL), cool to about −5° C., and treat dropwise with nitric acid (11.00 mL, 174 mmol) over 20 minutes. Allow reaction mixture to warm to RT and stir for 30 min. Pour onto crushed ice with stiffing and partition with tert-butyl methyl ether (MTBE) (200 mL). Separate the aqueous layer and extract with MTBE (2×50 mL). Combine organic layers, dry and concentrate under reduced pressure to provide 1-bromo-4-fluoro-2-methyl-5-nitrobenzene as an orange-colored viscous oil (39.0 g).
後処理
- customAllow reaction mixture
- additionPour
- customonto crushed ice with stiffing
- custompartition with tert-butyl methyl ether (MTBE) (200 mL)
- customSeparate the aqueous layer
- extractionextract with MTBE (2×50 mL)
- customCombine organic layers, dry
- concentrationconcentrate under reduced pressure
出典と根拠
- ORDレコード
- ord-11409640bb6745f38880db83dafaac01
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08741911B2
反応ノート
読み込み中…