HRID128447

反应详情

EQUATION

反应方程式

HRID 128447 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 0.71 g (4.0 mmole) of palladium chloride, 2.1 g (8.0 mmole) of triphenylphosphine, 0.80 g (4.2 mmole) of cuprous iodide, 68.8 g (0.20 mole) of 5-chloro-2-iodobenzophenone, 200 ml of diethylamine, and 400 ml of methylene chloride was stirred at room temperature under argon until complete solution was obtained. In one portion, 40.0 g (0.22 mole) of N-propargylphthalimide was added to the solution and the resulting mixture stirred for 20 hr. The volatiles were removed at reduced pressure and the residue was triturated with 200 ml of iospropanol. The resulting precipitate was collected by filtration to give crude end product. Recrystallization from acetone gave cream colored prisms, mp 148°-150° C.

WORKUP

后处理

  1. customwas obtained
  2. stirringthe resulting mixture stirred for 20 hr
  3. customThe volatiles were removed at reduced pressure
  4. customthe residue was triturated with 200 ml of iospropanol
  5. filtrationThe resulting precipitate was collected by filtration
  6. customto give crude end product
  7. customRecrystallization from acetone
  8. customgave cream colored prisms, mp 148°-150° C.