HRID1191680

反应详情

EQUATION

反应方程式

HRID 1191680 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

To a suspension of methyl 3-{[2-(2-hydroxy-3,3-dimethylbutyl)-4-methoxyphenylamino]methyl}benzoate (200 mg), 2-bromomesitylene (0.097 mL) and potassium carbonate (148 mg) in N,N-dimethylformamide (5 mL) was added tetrakis(triphenylphosphine)palladium (0) (31.1 mg) at room temperature, and this resulting mixture was stirred at 150° C. for 2 hours under an argon atmosphere. The reaction mixture was cooled to room temperature, diluted with water and extracted with ethyl acetate. The organic layer was washed with saturated saline, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluting solvent: ethyl acetate-hexane) to obtain the title compound (127 mg).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with saturated saline
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (eluting solvent: ethyl acetate-hexane)