Methanol → Methyl 3-acetyl-2-hydroxybenzoate

HRID 876541ノート

反応式

HRID 876541 の反応式
[C:1]([C:4]1[C:5]([OH:13])=[C:6]([CH:10]=[CH:11][CH:12]=1)[C:7]([OH:9])=[O:8])(=[O:3])[CH3:2].OS(O)(=O)=O.[CH3:19]O>>[C:1]([C:4]1[C:5]([OH:13])=[C:6]([CH:10]=[CH:11][CH:12]=1)[C:7]([O:9][CH3:19])=[O:8])(=[O:3])[CH3:2]

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 108992643-Acetyl-2-hydroxybenzoic acid

生成物 1

HCID 13037297Methyl 3-acetyl-2-hydroxybenzoate収率 20%

実験手順

To a solution of 3-acetyl-2-hydroxybenzoic acid 32 (3 g, 16.7 mmol) in MeOH (50 mL) was added conc. H2SO4 (3.0 mL. The reaction mixture was heated at reflux for 12 h. After concentration en vacuo, the crude residue was diluted with H2O, basified to pH=8 with aq NaHCO3 and extracted with EtOAc. The combined organic extracts were dried (MgSO4) and concentrated to give 38 as a white solid (550 mg, 20% yield).

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux for 12 h
  3. concentrationAfter concentration en vacuo
  4. additionthe crude residue was diluted with H2O
  5. extractionextracted with EtOAc
  6. dry with materialThe combined organic extracts were dried (MgSO4)
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-df360830e5a64d12a0d55b6271278789
出典データセット
uspto-grants-2015_03
特許番号
US08987258B2

反応ノート

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