HRID1191672

反应详情

EQUATION

反应方程式

HRID 1191672 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
160 °C

PROCEDURE

实验过程

A mixture of 1-(2-amino-4-chloro-5-methoxyphenyl)-3-methylpentan-2-ol (602 mg), tetrakis(triphenylphosphine)palladium (0) (135 mg), potassium carbonate (646 mg), 2-bromomesitylene (0.420 mL) and N,N-dimethylformamide (11.7 mL) was stirred at 160° C. for one hour under microwave irradiation. The reaction mixture was allowed to cool to ambient temperature. Water was added to the reaction mixture and this resulting mixture was extracted with ethyl acetate. The organic layer was washed with saturated saline, dried over anhydrous sodium 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 (514 mg).

WORKUP

后处理

  1. temperatureto cool to ambient temperature
  2. extractionthis resulting mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with saturated saline
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (eluting solvent: ethyl acetate-hexane)