Potassium Nitrate → 2,5-Difluoro-1-methyl-3-nitrobenzene

HRID 1857418노트

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HRID 1857418 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[CH3:9].[N+:10]([O-])([O-:12])=[O:11].[K+]>OS(O)(=O)=O>[F:1][C:2]1[C:7]([N+:10]([O-:12])=[O:11])=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[CH3:9]

참가 물질

4

반응물 2

HCID 24434Potassium NitrateHCID 679802,5-Difluorotoluene

생성물 1

HCID 552741502,5-Difluoro-1-methyl-3-nitrobenzene수율 91%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

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온도
28 °C

실험 절차

To a stirred solution of 2,5-difluorotoluene (0.544 g, 4.25 mmol, Aldrich, used as received) in conc. H2SO4 (5.0 mL) at 0° C., KNO3 (0.430 g, 4.25 mmol) was added in one portion. The resulting pale yellow solution was warmed to 28° C. and stirred at that temperature overnight. It was then poured into ice (25 g) and extracted with ethyl acetate (40 mL). The extract was dried over Na2SO4 and evaporated to afford 0.555 g (91%) of the title compound as a light red oil; 1H NMR (CDCl3): 2.369 (d, 3H, J=1.8 Hz), 7.127 (dd, 1H, J1 =8.1 Hz, J2 =6.0 Hz), 7.734 (dd, 1H, J1 =8.4 Hz, J2 =6.3 Hz).

후처리

  1. extractionextracted with ethyl acetate (40 mL)
  2. dry with materialThe extract was dried over Na2SO4
  3. customevaporated

출처 및 근거

ORD 기록
ord-7a81ac6fc04949d2aa53239f919dfa9e
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06147075

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