반응 #723013

ord-44ada84301f54113b404fe531e5ffc44

용매

반응 조건

온도
160°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타at −70° C.
  2. 2
    온도cooled
  3. 3
    기타Some of the solvent is removed
  4. 4
    기타a rotary evaporator
  5. 5
    여과the resulting precipitate is filtered off with suction
  6. 6
    기타recrystallized from ethanol

실험 절차

50.0 g of 3,4-dimethoxy-ω-nitrostyrene and 1.0 g (9.1 mmol) of hydroquinone are suspended in 200 ml of abs. toluene and, at −70° C., admixed with 55.0 g (1.02 mol) of liquid 1,3-butadiene. The mixture is stirred in an autoclave at 160° C. for 6 days and then cooled. Some of the solvent is removed using a rotary evaporator, and the resulting precipitate is filtered off with suction and recrystallized from ethanol. M.p.: 113.5-115.5° C.; Yield 76.3% of Th.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06191138B1uspto-grants-2001_02