Methanol → Methyl 2,3,4-trimethoxybenzoate

HRID 1057946

反応式

HRID 1057946 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].S(=O)(=O)(O)O.[CH3:21]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][CH3:21])=[O:6]

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 113082,3,4-Trimethoxybenzoic acid

生成物 1

HCID 13940801Methyl 2,3,4-trimethoxybenzoate

反応条件

温度
80 °C

実験手順

2,3,4-trimethoxybenzoic acid (7.3 g) was dissolved in methanol (73 ml), mixed with sulfuric acid (15 ml), and stirred for 3 hours while heating at 80° C. The resultant was allowed to stand for cooling, evaporated under reduced pressure for removing the solvent, and the residue was added to cold water, followed by extraction with ethyl acetate. The organic layer was washed with saturated sodium bicarbonate water and then with a saturated aqueous sodium chloride solution, dried over sodium sulfate anhydride, and evaporated under reduced pressure for removing the solvent to give Compound IIbt-a (6.8 g, 87%) as a colorless oily substance.

後処理

  1. temperaturefor cooling
  2. customevaporated under reduced pressure
  3. customfor removing the solvent
  4. additionthe residue was added to cold water
  5. extractionfollowed by extraction with ethyl acetate
  6. washThe organic layer was washed with saturated sodium bicarbonate water
  7. dry with materialwith a saturated aqueous sodium chloride solution, dried over sodium sulfate anhydride
  8. customevaporated under reduced pressure
  9. customfor removing the solvent
  10. customto give Compound IIbt-a (6.8 g, 87%) as a colorless oily substance

出典と根拠

ORDレコード
ord-02da7c6493834e3c8659638193a9176f
出典データセット
uspto-grants-2003_02
特許番号
US06514996B2

関連ノート

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