Potassium Nitrate → 1-Chloro-2,5-difluoro-4-nitrobenzene
反応式
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[F:9].[N+:10]([O-])([O-:12])=[O:11].[K+]>OS(O)(=O)=O>[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([N+:10]([O-:12])=[O:11])=[CH:4][C:3]=1[F:9]参加物
4
実験手順
To a stirred solution of 1-chloro-2,5-difluorobenzene (0.770 g, 5.18 mmol) in concd H2SO4 (8.0 mL) at 0° C., KNO3.(0.525 g, 5.19 mmol) was added in one lot. The resulting yellow solution was allowed to warm to room temperature and stirred overnight at room temperature. It was then poured into ice (80 g) and extracted with ethyl acetate (75 mL). The ethyl acetate was dried over anhydrous Na2SO4, removed under vacuum and the residue was dried further under vacuum to afford 0.845 g (85%) of title compound as a yellow liquid; 1H NMR (CDCl3) δ 7.43 (dd, 1H, J1=9.6 Hz, J2=6.0 Hz), 7.93 (t, 1H, J=7.2 Hz).
後処理
- customat 0° C.
- addition(0.525 g, 5.19 mmol) was added in one lot
- extractionextracted with ethyl acetate (75 mL)
- dry with materialThe ethyl acetate was dried over anhydrous Na2SO4
- customremoved under vacuum
- customthe residue was dried further under vacuum
出典と根拠
- ORDレコード
- ord-5c195ed4940a49aab094b7143c470784
- 出典データセット
- uspto-grants-2001_06
- 特許番号
- US06251903B1
反応ノート
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