HRID2167664

反应详情

EQUATION

反应方程式

HRID 2167664 的结构方程式

PROCEDURE

实验过程

To a solution of triethyl((4-(methoxymethoxy)-2-methylphenyl)ethynyl)silane (1.0 equiv.) at 0° C. was slowly added tetrabutylammonium fluoride (1M solution in THF, 0.20 equiv.). At this point, the ice-bath was removed and the reaction mixture was allowed to stir at room temperature for 45 minutes. The reaction mixture was then passed through a pad of silica (packed with hexane) and eluted with 20% EtOAc in Hexanes to remove insoluble salts. The crude product was then purified by Combiflash using 0-10% EtOAc in Hexanes to give 1-ethynyl-4-(methoxymethoxy)-2-methylbenzene (6-8) as a slightly brown liquid.

WORKUP

后处理

  1. customat 0° C.
  2. customAt this point, the ice-bath was removed
  3. washeluted with 20% EtOAc in Hexanes
  4. customto remove insoluble salts
  5. customThe crude product was then purified by Combiflash