Potassium Nitrate → 1-Bromo-2,4-difluoro-5-nitrobenzene

HRID 439531

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HRID 439531 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[F:9].[N+:10]([O-])([O-:12])=[O:11].[K+]>OS(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[F:9]

참가 물질

4

반응물 2

HCID 24434Potassium NitrateHCID 676741-Bromo-2,4-difluorobenzene

생성물 1

HCID 2230781-Bromo-2,4-difluoro-5-nitrobenzene수율 91.3%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

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온도
28 °C

실험 절차

To a stirred solution of 1-bromo-2,4-difluorobenzene (0.512 g, 2.65 mmol, Aldrich, used as received) in conc. H2SO4 (5.0 mL) at 0° C., KNO3 (0.275 g, 2.72 mmol) was added in one portion. The resulting solution was allowed to warm to 28° C. and was stirred at that temperature overnight. It was then poured into ice (50 g) and extracted with ethylacetate (50 mL). The extract was dried over Na2SO4, and evaporated to afford 0.576 g (91%) pure title compound as light red oil; 1H NMR (CDCl3); δ7.141 (dd, 1H, J1 10.2 Hz, J2 =7.8 Hz), 8.375 (t, 1H, J=7.5 Hz).

후처리

  1. extractionextracted with ethylacetate (50 mL)
  2. dry with materialThe extract was dried over Na2SO4
  3. customevaporated

출처 및 근거

ORD 기록
ord-745959f1cc00461f8b1ed9db387be198
출처 데이터셋
uspto-grants-1996_05
특허 번호
US05514680

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