2,3-Dihydroxybenzoic Acid → Ethyl 2,3-dihydroxybenzoate

HRID 383904

反応式

HRID 383904 の反応式
[OH:1][C:2]1[C:10]([OH:11])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[CH2:17](O)[CH3:18]>>[OH:1][C:2]1[C:10]([OH:11])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([O:6][CH2:17][CH3:18])=[O:5]

参加物

4

反応物 3

HCID 192,3-Dihydroxybenzoic AcidHCID 702EthanolHCID 1118Sulfuric Acid

生成物 1

HCID 2779843Ethyl 2,3-dihydroxybenzoate収率 100%

実験手順

To a solution of 2,3-dihydroxybenzoic acid (25 g) in ethanol (320 ml) was added concentrated sulfuric acid (1.8 ml), and the mixture was heated under reflux for one day. The reaction mixture was concentrated, poured into water, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to normal phase chromatography (elution solvent ethyl acetate) to give the title compound (30 g, 100%).

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for one day
  3. concentrationThe reaction mixture was concentrated
  4. additionpoured into water
  5. extractionthe mixture was extracted with ethyl acetate
  6. washThe organic layer was washed with saturated brine
  7. dry with materialdried over sodium sulfate
  8. customThe solvent was evaporated under reduced pressure
  9. washThe residue was subjected to normal phase chromatography (elution solvent ethyl acetate)

出典と根拠

ORDレコード
ord-e38d34a083614660b0d3bfd1ce15e04d
出典データセット
uspto-grants-2013_02
特許番号
US08367695B2

関連ノート

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