HRID385032

反应详情

EQUATION

反应方程式

HRID 385032 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

Methyl 3-t-butyl-5-iodo-4-methoxybenzoate (2.77 g) was dissolved in N,N-dimethylformamide (30 mL), and copper cyanide (965 mg) was added to the solution, and then the mixture was stirred at 150° C. for 2.5 hours. To the reaction solution, 10% potassium carbonate was added, and then the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the obtained residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=3:1) to obtain the title compound (1.48 g) as a yellow oily substance.

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with water and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled off under reduced pressure
  5. customthe obtained residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=3:1)