HRID660612

反应详情

EQUATION

反应方程式

HRID 660612 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2,6-dihydroxybenzoic acid (500 mg, 3.24 mmol) in ethanol (8 mL) is added NaOH (130 mg, 3.24 mmol). After the mixture is stirred at RT for 3 h, the solvent is removed under reduced pressure. The resulting sodium salt is dissolved in DMF (10 mL) then benzyl bromide (0.39 mL, 3.24 mmol) is added and the mixture is stirred at RT for 18 h. Water is added and the mixture is extracted with EtOAc. The organic phase is washed with water and brine then is dried over sodium sulfate. The solvent is removed under reduced pressure and the residue is purified by flash chromatography using hexane/EtOAc (10:1) as eluent to give the title compound as an oil.

WORKUP

后处理

  1. customthe solvent is removed under reduced pressure
  2. dissolutionThe resulting sodium salt is dissolved in DMF (10 mL)
  3. stirringthe mixture is stirred at RT for 18 h
  4. extractionthe mixture is extracted with EtOAc
  5. washThe organic phase is washed with water and brine
  6. dry with materialthen is dried over sodium sulfate
  7. customThe solvent is removed under reduced pressure
  8. customthe residue is purified by flash chromatography