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

HRID 489141

反応式

HRID 489141 の反応式
[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]

参加物

4

反応物 3

HCID 192,3-Dihydroxybenzoic AcidHCID 887MethanolHCID 1118Sulfuric Acid

生成物 1

HCID 75484Methyl 2,3-Dihydroxybenzoate

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-ee1b46de3f4c429aa2531db13f266d31
出典データセット
uspto-grants-2005_12
特許番号
US06977255B2

関連ノート

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