HRID240273

反应详情

EQUATION

反应方程式

HRID 240273 的结构方程式

PROCEDURE

实验过程

To a solution of 2-bromo-5-fluorobenzoic acid (9) (21.90 g, 100 mmol) in methanol (100 mL) was added conc. H2SO4 (2 mL). The mixture was heated at reflux for 21 h. Most of the solvent was evaporated and diluted with water (200 mL). The mixture was extracted with EtOAc (150 mL×2). The combined extracts were washed with saturated NaHCO3 and brine, dried over MgSO4, and concentrated to give methyl 2-bromo-5-fluorobenzoate (10).

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 21 h
  3. customMost of the solvent was evaporated
  4. additiondiluted with water (200 mL)
  5. extractionThe mixture was extracted with EtOAc (150 mL×2)
  6. washThe combined extracts were washed with saturated NaHCO3 and brine
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated