反应 #84254

ord-cd850f646e874edab909d8c8af2c313c

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 through celite
  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 5.00 g of 1-(3,5-dichloropyridin-2-yl)ethanone in 75 ml of tetrahydrofuran, 9.94 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 through celite, 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 5:95 to 15:85) as the eluent to obtain 6.64 g of the desired product as a brown oil.

来源

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