Nitric Acid → 1-Chloro-4,5-difluoro-2-nitrobenzene
반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[C:4]([F:9])[CH:3]=1.OS(O)(=O)=O.[N+:15]([O-])([OH:17])=[O:16]>>[Cl:1][C:2]1[CH:3]=[C:4]([F:9])[C:5]([F:8])=[CH:6][C:7]=1[N+:15]([O-:17])=[O:16]참가 물질
4
실험 절차
To a flask was added 4-chloro-1,2-difluorobenzene (8.97 g, 60.4 mmol), followed by adding 98% con. H2SO4 (16.1 mL, 302 mmol) and 65% con. HNO3 (5.0 mL, 66.4 mmol) at 0° C. The mixture was stirred at rt for 5 hours, then poured into ice water (500 mL). The resulted mixture was extracted with ethyl acetate (200 mL×3). The combined organic phase were washed with saturated aqueous NaHCO3 solution (200 mL×2) and brine (200 mL), dried over anhydrous Na2SO4, and concentrated in vacuo to give the title compound as yellow liquid (11.31 g, 96.7%).
후처리
- additionby adding 98% con
- customat 0° C
- extractionThe resulted mixture was extracted with ethyl acetate (200 mL×3)
- washThe combined organic phase were washed with saturated aqueous NaHCO3 solution (200 mL×2) and brine (200 mL)
- dry with materialdried over anhydrous Na2SO4
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-b51a08a62c8f412b80f03d07f4fab644
- 출처 데이터셋
- uspto-grants-2016_05
- 특허 번호
- US09326975B2
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