Ethanol → 2-(Ethoxycarbonyl)-6-nitrobenzoic acid

HRID 494330노트

반응식

HRID 494330 반응식
[N+:1]([C:4]1[CH:12]=[CH:11][CH:10]=[C:6]([C:7]([OH:9])=[O:8])[C:5]=1[C:13]([OH:15])=[O:14])([O-:3])=[O:2].S(=O)(=O)(O)O.[CH2:21](O)[CH3:22]>>[C:13]([C:5]1[C:4]([N+:1]([O-:3])=[O:2])=[CH:12][CH:11]=[CH:10][C:6]=1[C:7]([O:9][CH2:21][CH3:22])=[O:8])([OH:15])=[O:14]

참가 물질

4

반응물 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 690433-Nitrophthalic acid

생성물 1

HCID 120189282-(Ethoxycarbonyl)-6-nitrobenzoic acid

실험 절차

A mixture of 3-nitrophthalic acid (35 g) in ethanol (300 ml) containing conc. sulfuric acid (20 ml) was heated under reflux for 24 hours. The solvent was evaporated in vacuo and the residue was poured into cold water (700 ml). The mixture was extracted with ethyl acetate. The organic layer was washed with water and shaken with an aqueous solution of potassium carbonate. The aqueous layer was made acidic with hydrochloric acid and the mixture was extracted with methylene chloride. The organic layer was washed with water, then dried, followed by evaporation of the solvent. The resultant solid (29 g, 74%) was used for the subsequent reaction without purification.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 24 hours
  3. customThe solvent was evaporated in vacuo
  4. additionthe residue was poured into cold water (700 ml)
  5. extractionThe mixture was extracted with ethyl acetate
  6. washThe organic layer was washed with water
  7. extractionthe mixture was extracted with methylene chloride
  8. washThe organic layer was washed with water
  9. customdried
  10. customfollowed by evaporation of the solvent
  11. customThe resultant solid (29 g, 74%) was used for the subsequent reaction without purification

출처 및 근거

ORD 기록
ord-9f000dff8544489296e6193b0ec1e367
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07538133B2

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