HRID876541

反应详情

EQUATION

反应方程式

HRID 876541 的结构方程式

PROCEDURE

实验过程

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).

WORKUP

后处理

  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