HRID591465

反应详情

EQUATION

反应方程式

HRID 591465 的结构方程式

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a mixture of (7-chloro-6-hydroxy-1-benzofuran-3-yl)acetic acid (1.65 g) and MeOH (40 mL) was added conc. H2SO4 (0.078 mL). The mixture was stirred at 60° C. for 3 h. The mixture was concentrated in vacuo. The residue was neutralized with saturated aqueous NaHCO3 and extracted with EtOAc. The organic layer was washed with brine, dried over MgSO4, and concentrated in vacuo. The residue was dissolved in toluene and hexane. The insoluble material was filtered and washed with toluene and hexane. The filtrate was purified by silica gel column chromatography (EtOAc/hexane) to give the title compound (1.49 g).

WORKUP

后处理

  1. concentrationThe mixture was concentrated in vacuo
  2. extractionextracted with EtOAc
  3. washThe organic layer was washed with brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo
  6. dissolutionThe residue was dissolved in toluene
  7. filtrationThe insoluble material was filtered
  8. washwashed with toluene and hexane
  9. customThe filtrate was purified by silica gel column chromatography (EtOAc/hexane)