Methanol → Methyl 2,3,4-trimethoxybenzoate

HRID 1156020

反応式

HRID 1156020 の反応式
[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]

参加物

4

反応物 2

HCID 887MethanolHCID 113082,3,4-Trimethoxybenzoic acid

生成物 1

HCID 13940801Methyl 2,3,4-trimethoxybenzoate

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-1bfa41ab78304895b1b8beb822f51a13
出典データセット
uspto-grants-1982_06
特許番号
US04333937

関連ノート

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