HRID1271038

反应详情

EQUATION

反应方程式

HRID 1271038 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 5.6 mL of 1-ethyl-4-iodobenzene, 75 mL of triethylamine, 6 mL of trimethylsilylacetylene, 0.49 g of dichlorotriphenylphosphine palladium II and 0.314 g copper iodide was magnetically stirred at ambient temperature for 18 hrs. The thick dark brown mixture was filtered, washing the gray precipitate with hexanes. The filtrate and washings were evaporated in vacuo and the residue dissolved in hexanes. This solution was 96.7% pure by GC analysis. The solution was passed down a column of silica gel which had been equilibrated in the same solvent and the eluates evaporated in vacuo to yield 9.3 g of 4-ethyl-1-trimethylsilyl ethynylbenzene as a dark amber liquid.

WORKUP

后处理

  1. filtrationThe thick dark brown mixture was filtered
  2. washwashing the gray precipitate with hexanes
  3. customThe filtrate and washings were evaporated in vacuo
  4. dissolutionthe residue dissolved in hexanes
  5. customthe eluates evaporated in vacuo