2,3-Dihydroxybenzoic Acid → Methyl 2,3-Dihydroxybenzoate

HRID 489141

반응식

HRID 489141 반응식
[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.[CH3:17]O>>[OH:1][C:2]1[C:10]([OH:11])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([O:6][CH3:17])=[O:5]

참가 물질

4

실험 절차

A mixture of 2,3-dihydroxybenzoic acid (3.8 g, 24.6 mmol) in methanol (300 ml) was treated dropwise with conc. Sulfuric acid (4.2 g) and the resultant solution was heated at reflux temperature overnight. Upon cooling the solvent was evaporated and the residue poured into ice-water. The mixture was extracted with dichloromethane (3×50 ml) and the combined organic fractions dried (Na2SO4) and concentrated to yield a pale tan solid (4.05 g).

후처리

  1. temperatureat reflux temperature overnight
  2. temperatureUpon cooling the solvent
  3. customwas evaporated
  4. additionthe residue poured into ice-water
  5. extractionThe mixture was extracted with dichloromethane (3×50 ml)
  6. dry with materialthe combined organic fractions dried (Na2SO4)
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ee1b46de3f4c429aa2531db13f266d31
출처 데이터셋
uspto-grants-2005_12
특허 번호
US06977255B2

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