HRID2354143

反应详情

EQUATION

反应方程式

HRID 2354143 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

0.32 g (1.2 mmol, purity 99%) triphenylphosphine, 0.085 g (0.12 mmol, purity 99%) bis-triphenylphosphine palladium dichloride, and 0.14 g (0.72 mmol, purity 98%) copper(I)iodide are added to a mixture of 56.8 g (0.24 mol, purity 98%) N-(2-bromo-4-fluorophenyl)acetamide, 30.9 g (0.264 mol, purity 98%) 2-methylbut-3-yn-2-ol and 121.4 g (1.2 mol) triethylamine and the mixture is heated for 6 hours while stirring at 85° C. The surplus triethylamine is distilled off in a vacuum, approximately 170 ml toluene is added, the same quantity of water is added, and the phases are separated at ˜70° C.

WORKUP

后处理

  1. temperaturethe mixture is heated for 6 hours
  2. distillationThe surplus triethylamine is distilled off in a vacuum, approximately 170 ml toluene
  3. additionis added
  4. additionthe same quantity of water is added
  5. customthe phases are separated at ˜70° C.