HRID1884244

反应详情

EQUATION

反应方程式

HRID 1884244 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of 5.00 g (29.3 mmol) of (4-chlorophenyl)acetic acid, 5.23 g (43.9 mmol) of thionyl chloride and 50 ml of toluene was stirred at 50° C. for 30 minutes and then 80° C. for 2.5 hours, cooled and concentrated under reduced pressure. The residue was added to a mixture of 5.18 g (28.5 mmol) 2-(3,4-dimethoxyphenyl)ethylamine, 3.46 g (34.2 mmol) of triethylamine and 50 ml tetrahydrofuran at 0° C. and kept at 0° C. for 30 minutes and at room temperature for 3 hours. Water and ethyl acetate were added to the reaction mixture and precipitated solid was collected with filtration. The obtained solid was dried to give 5.75 g of N-[2-(3,4-dimethoxyphenyl)ethyl]-2-(4-chlorophenyl) acetamide.

WORKUP

后处理

  1. wait80° C. for 2.5 hours
  2. temperaturecooled
  3. concentrationconcentrated under reduced pressure
  4. waitkept at 0° C. for 30 minutes and at room temperature for 3 hours
  5. customprecipitated solid
  6. filtrationwas collected with filtration
  7. customThe obtained solid was dried