HRID1859275

反应详情

EQUATION

反应方程式

HRID 1859275 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

0.25 g (1.1 mmol) of palladium(II) acetate and 1.16 g (4.4 mmol) of triphenylphosphine are introduced into 100 ml of dichloromethane in a 250 ml round-bottomed flask under argon. The yellow solution is stirred at room temperature for 1 h. Then 0.06 g (0.5 mmol) of 4-dimethylaminopyridine, 8.53 g (55.5 mmol) of 1,2,2,6,6-pentamethylpiperidine and 5.1 g (50 mmol) of phenylacetylene are added. The mixture is heated to reflux at 40° C. and then 6.83 g (50 mmol) of n-butyl chloroformate are added dropwise over the course of 1 h. After a reaction time of 20 h, the reaction mixture is worked up by distillation to isolate n-butyl phenylpropynoate in 85% yield.

WORKUP

后处理

  1. temperatureThe mixture is heated
  2. temperatureto reflux at 40° C.
  3. distillationAfter a reaction time of 20 h, the reaction mixture is worked up by distillation