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

HRID 653709

반응식

HRID 653709 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 acid수율 74%

실험 절차

A solution of 3-nitrophthalic acid (35 g) in ethanol (300 ml) containing conc. sulfuric acid (20 ml) was heated for 24 hours under reflux. The solvent was distilled off, and the residue was poured into ice-water (700 ml), which was extracted with ethyl acetate. The organic layer was washed with water, which was extracted with an aqueous solution of potassium carbonate. The aqueous layer was made acidic with hydrochloric acid, followed by extraction with methylene chloride. The organic layer was washed with water and dried. The solvent was distilled off to give a solid product (29 g, 74%), which was used in the subsequent reaction without purification.

후처리

  1. temperaturewas heated for 24 hours
  2. temperatureunder reflux
  3. distillationThe solvent was distilled off
  4. additionthe residue was poured into ice-water (700 ml), which
  5. extractionwas extracted with ethyl acetate
  6. washThe organic layer was washed with water, which
  7. extractionwas extracted with an aqueous solution of potassium carbonate
  8. extractionfollowed by extraction with methylene chloride
  9. washThe organic layer was washed with water
  10. customdried
  11. distillationThe solvent was distilled off

출처 및 근거

ORD 기록
ord-6c0f696732694d07bf881e6f3f1308d7
출처 데이터셋
uspto-grants-1992_07
특허 번호
US05128356

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