반응 #591533

ord-60946d5b91594f25bfc750fe1dd0a0ec

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출was extracted with ethyl ether (4×50 mL)
  2. 2
    세척The combined organic phase was washed with HCl aqueous solution (1N, 20 mL) and brine (2×30 mL) successively
  3. 3
    건조dried over Na2SO4
  4. 4
    여과filtered
  5. 5
    농축concentrated under reduced pressure
  6. 6
    기타was directly used in the next step without further purification

실험 절차

Sodium hydroxide (50% aqueous solution, 29.3 g, 0.505 mol) was added to a mixture of 4-bromo-benzeneacetonitrile (9.80 g, 0.0500 mol), benzyltriethylammonium chloride (0.90 g, 0.0040 mol), ethane, and 1-bromo-2-chloro-(14.5 g, 0.101 mol) at 50° C. overnight. The mixture was poured into ice-water (80 mL) and was extracted with ethyl ether (4×50 mL). The combined organic phase was washed with HCl aqueous solution (1N, 20 mL) and brine (2×30 mL) successively, dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was the desired product, which was directly used in the next step without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07776874B2uspto-grants-2010_08