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

HRID 494330

反応式

HRID 494330 の反応式
[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]

参加物

4

反応物 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 690433-Nitrophthalic acid

生成物 1

HCID 120189282-(Ethoxycarbonyl)-6-nitrobenzoic acid

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9f000dff8544489296e6193b0ec1e367
出典データセット
uspto-grants-2009_05
特許番号
US07538133B2

関連ノート

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