反応 #2507833

ord-0a742841cf404074ab18670d412b94fc

反応方程式

CCCCCC1COc2cc(C=CC3=Cc4cc(F)cc(F)c4OC3)c(F)cc2C1
6,8-Difluoro-3-[2-(6-fluoro-3-pentylchroman-7-yl)vinyl]-2H-chromene
CCCCCC1COc2cc(CCC3=Cc4cc(F)cc(F)c4OC3)c(F)cc2C1
6,8-Difluoro-3-[2-(6-fluoro-3-pentylchroman-7-yl)ethyl]-2H-chromene

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The catalyst is filtered off
  2. 2
    その他the solution is evaporated
  3. 3
    ろ過the residue is filtered through silica gel with toluene/heptane (3:2)
  4. 4
    その他the crude product is recrystallised from n-heptane at −25° C.
  5. 5
    その他giving colourless crystals of m.p. 84° C.

実験手順

6,8-Difluoro-3-[2-(6-fluoro-3-pentylchroman-7-yl)vinyl]-2H-chromene is dissolved in THF and hydrogenated to completion on a palladium/active carbon catalyst. The catalyst is filtered off, the solution is evaporated, the residue is filtered through silica gel with toluene/heptane (3:2), and the crude product is recrystallised from n-heptane at −25° C., giving colourless crystals of m.p. 84° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07955664B2uspto-grants-2011_06