HRID8377

反应详情

EQUATION

反应方程式

HRID 8377 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

The product of Step A (1.8 g) in dry acetonitrile (40 mL) was treated sequentially with tetrakis(triphenylphosphine)palladium(0) (0.1 g), triethylamine (1.27 g), and CuI (10 mg) then heated at 60° C. for 30 minutes. The mixture was cooled to ambient temperature, treated with 3-butyn-1-ol (0.361 g) and heated at reflux temperature for 18 hours. The mixture was cooled to ambient temperature and evaporated to dryness. The residue was crystallized, twice, from acetone to afford the title compound (1.02 g).

WORKUP

后处理

  1. temperatureThe mixture was cooled to ambient temperature
  2. temperatureheated
  3. temperatureat reflux temperature for 18 hours
  4. temperatureThe mixture was cooled to ambient temperature
  5. customevaporated to dryness
  6. customThe residue was crystallized