Methanol → Methyl 2,3,4-trimethoxybenzoate

HRID 1156020

반응식

HRID 1156020 반응식
[CH3:1][O:2][C:3]1[C:11]([O:12][CH3:13])=[C:10]([O:14][CH3:15])[CH:9]=[CH:8][C:4]=1[C:5]([OH:7])=[O:6].[CH3:16]O>S(=O)(=O)(O)O>[CH3:1][O:2][C:3]1[C:11]([O:12][CH3:13])=[C:10]([O:14][CH3:15])[CH:9]=[CH:8][C:4]=1[C:5]([O:7][CH3:16])=[O:6]

참가 물질

4

반응물 2

HCID 887MethanolHCID 113082,3,4-Trimethoxybenzoic acid

생성물 1

HCID 13940801Methyl 2,3,4-trimethoxybenzoate

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

To a solution of 2,3,4-trimethoxybenzoic acid (25 g) in dry methanol (250 ml), concentrated sulfuric acid (2.4 ml) was added. The reaction solution was refluxed for 20 hr, concentrated to half its volume by evaporation, and poured into a mixture of ice and water. The solution was extracted with methylene chloride and the organic extract was washed with cold aqueous sodium carbonate solution and water, dried over sodium sulfate and evaporated to give 25.4 g of 2,3,4-trimethoxybenzoic acid, methyl ester: ir (CHCl3) 1720 cm-1 ; and nmr (CDCl3) δ 3.85 (s, 3H), 3.87 (s, 3H), 3.92 (s, 6H), 6.65 (d, 1H) and 7.55 (d, 1H).

후처리

  1. temperatureThe reaction solution was refluxed for 20 hr
  2. concentrationconcentrated to half its volume by evaporation
  3. additionpoured into a mixture of ice and water
  4. extractionThe solution was extracted with methylene chloride
  5. extractionthe organic extract
  6. washwas washed with cold aqueous sodium carbonate solution and water
  7. dry with materialdried over sodium sulfate
  8. customevaporated

출처 및 근거

ORD 기록
ord-1bfa41ab78304895b1b8beb822f51a13
출처 데이터셋
uspto-grants-1982_06
특허 번호
US04333937

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