HRID2232964

反应详情

EQUATION

反应方程式

HRID 2232964 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

1,2-Dichloro-3-iodobenzene (4.95 g, 18.1 mmol), trimethylsilylacetylene (2 g, 20 mmol), bis(triphenylphosphine)palladium(II)chloride (245 mg, 0.35 mmol), and copper(I)iodide (45 mg, 0.24 mmol) were combined in triethylamine (120 mL) and heated at reflux for 45 minutes. The mixture was allowed to cool to room temperature and was then partitioned between diethyl ether and saturated sodium chloride. The organic phase was dried with sodium sulfate, filtered through celite, and the filtrate was concentrated under reduced pressure. The residue was taken directly on to the next step.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 45 minutes
  3. customwas then partitioned between diethyl ether and saturated sodium chloride
  4. dry with materialThe organic phase was dried with sodium sulfate
  5. filtrationfiltered through celite
  6. concentrationthe filtrate was concentrated under reduced pressure