HRID1873962

反应详情

EQUATION

反应方程式

HRID 1873962 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Methyl 2-fluoro-4-hydroxybenzoate (1.4685 g, manufactured by Changzhou Fine Chemical Corp.) and potassium carbonate (3.6917 g; manufactured by Sigma-Aldrich Co.) were suspended in dehydrated DMF (21 mL; manufactured by Kanto Chemical Co., Inc.), added with benzyl bromide (1.22 mL; manufactured by Wako Pure Chemical Industries, Ltd.), and stirred at 50° C. overnight. After cooling to the room temperature, it was added to water and extraction was carried out twice with ethyl acetate. The organic layer was washed twice with water and once with brine and dried over anhydrous sodium sulfate. After the solvent was evaporated under reduced pressure, the residue was purified by column chromatography (“COLUMN-B”; n-hexane:ethyl acetate=97:3→77:23) to obtain the title compound (2.2207 g).

WORKUP

后处理

  1. temperatureAfter cooling to the room temperature, it
  2. washThe organic layer was washed twice with water and once with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customAfter the solvent was evaporated under reduced pressure
  5. customthe residue was purified by column chromatography (“COLUMN-B”; n-hexane:ethyl acetate=97:3→77:23)