Nitric Acid → 2,6-Dimethyl-3-nitrobenzoic acid

HRID 485540

반응식

HRID 485540 반응식
S(=O)(=O)(O)O.[N+:6]([O-:9])(O)=[O:7].[CH3:10][C:11]1[CH:19]=[CH:18][CH:17]=[C:16]([CH3:20])[C:12]=1[C:13]([OH:15])=[O:14]>C(Cl)Cl>[CH3:10][C:11]1[C:19]([N+:6]([O-:9])=[O:7])=[CH:18][CH:17]=[C:16]([CH3:20])[C:12]=1[C:13]([OH:15])=[O:14]

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 1118Sulfuric AcidHCID 124392,6-Dimethylbenzoic acid

생성물 1

HCID 2393292,6-Dimethyl-3-nitrobenzoic acid

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 46 ml of concentrated sulfuric acid and 23.5 ml of concentrated nitric acid was added slowly to a stirred solution of 2,6-dimethylbenzoic acid (50.0 g, 0.333 mole) in 200 ml of methylene chloride at a rate such that a gentle reflux was maintained throughout the addition. After complete addition, reflux was maintained for 30 minutes. The reaction mixture was cooled, poured onto 300 g of ice and the organic phase separated. The aqueous phase was extracted with three 200 ml portions of diethyl ether, and the organic phases were combined, dried over anhydrous magnesium sulfate, and filtered. The solvent was removed from the filtrate under reduced pressure to give 2,6-dimethyl-3-nitrobenzoic acid (60.2 g) as a solid.

후처리

  1. temperaturea gentle reflux
  2. temperaturewas maintained throughout the addition
  3. additionAfter complete addition
  4. temperaturereflux
  5. temperaturewas maintained for 30 minutes
  6. temperatureThe reaction mixture was cooled
  7. customthe organic phase separated
  8. extractionThe aqueous phase was extracted with three 200 ml portions of diethyl ether
  9. dry with materialdried over anhydrous magnesium sulfate
  10. filtrationfiltered
  11. customThe solvent was removed from the filtrate under reduced pressure

출처 및 근거

ORD 기록
ord-54fe3c46726b4aaca4c32bb2c93a68f1
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04536591

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