Potassium Nitrate → 4-tert-Butyl-1-fluoro-2-nitrobenzene

HRID 742339

반응식

HRID 742339 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([CH3:11])([CH3:10])[CH3:9])=[CH:4][CH:3]=1.[N+:12]([O-])([O-:14])=[O:13].[K+]>S(=O)(=O)(O)O>[C:8]([C:5]1[CH:6]=[CH:7][C:2]([F:1])=[C:3]([N+:12]([O-:14])=[O:13])[CH:4]=1)([CH3:11])([CH3:10])[CH3:9]

참가 물질

4

반응물 2

HCID 24434Potassium NitrateHCID 1365401-(1,1-Dimethylethyl)-4-fluorobenzene

생성물 1

HCID 227418934-tert-Butyl-1-fluoro-2-nitrobenzene수율 58.6%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

1-Fluoro-4-t-butylbenzene (10 g, 65.79 mmol) was dissolved in concentrated sulfuric acid (40 ml) at 0° C. Solid potassium nitrate (6.64 g, 65.79 mmol) was added in small portions during 1 hour. The temperature was kept below 5° C. Following the addition stirring was continued for 2 hours. The reaction mixture was poured into ice-water (400 ml) and extracted with dichloromethane (3×50 ml). The organic phase was washed with water, aqueous sodium bicarbonate (1M) and water successively, dried over MgSO4 and filtered through silica gel (5 g). Evaporation of solvent left the crude product (10.32 g). Column chromatography on silica gel using petroleum ether containing 1% dichloromethane as the eluent afforded the pure product (7.6 g colorless oil).

후처리

  1. customwas kept below 5° C
  2. additionthe addition
  3. extractionextracted with dichloromethane (3×50 ml)
  4. washThe organic phase was washed with water, aqueous sodium bicarbonate (1M) and water successively
  5. dry with materialdried over MgSO4
  6. filtrationfiltered through silica gel (5 g)
  7. customEvaporation of solvent
  8. waitleft the crude product (10.32 g)

출처 및 근거

ORD 기록
ord-cbba43a27d6b4d208a3824f53c01bab3
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05554630

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