Methanol → Methyl 2,3,4-trimethoxybenzoate

HRID 1057946

반응식

HRID 1057946 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].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]

참가 물질

4

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온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-02da7c6493834e3c8659638193a9176f
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06514996B2

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