反应 #84283

ord-41bd32319c9141c3a2e89490c2af54d8

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他After completion of the reaction
  2. 2
    过滤the precipitated solid was filtered off
  3. 3
    其他the solvent was evaporated under reduced pressure
  4. 4
    其他The resulting residue was purified by silica gel column chromatography

实验过程

To 0.90 g of 1-(3-chloro-5-methoxypyridin-2-yl)ethanone in 10 ml of tetrahydrofuran, 1.82 g of trimethylphenylammonium tribromide was added, and the mixture was stirred at room temperature for 16 hours. After completion of the reaction, the precipitated solid was filtered off, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography using ethyl acetate-hexane (with a gradient of from 1:9 to 3:7) as the eluent to obtain 0.57 g of the desired product as pale yellow crystals.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09434684B2uspto-grants-2016_09