반응 #60035

ord-8a00c94f26fa44bab243eb0d727978c8

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과After filtering off a solid impurity
  2. 2
    기타the aqueous layer was removed
  3. 3
    세척The organic layer was washed sequentially with water (60 ml), sat. aq. NaHCO3 (60 ml), water (60 ml), brine (60 ml)
  4. 4
    건조dried with Na2SO4
  5. 5
    여과filtered
  6. 6
    농축concentrated under reduced pressure
  7. 7
    기타The dark colored oil was dried overnight in vacuo

실험 절차

A stirred solution of 4-(2-chloroacetyl)benzenecarbonitrile (0.5 M) and imidazole (1.5 M) in CH3CN (200 ml) were heated for 14 hours at 60° C. The product was stripped of solvent under reduced pressure. The residue was diluted with dichloromethane (250 ml) and water (100 ml), and the mixture was stirred for 30 min. After filtering off a solid impurity, the aqueous layer was removed and discarded. The organic layer was washed sequentially with water (60 ml), sat. aq. NaHCO3 (60 ml), water (60 ml), brine (60 ml), dried with Na2SO4, filtered, and concentrated under reduced pressure. The dark colored oil was dried overnight in vacuo giving 4-(2-imidazolylacetyl)benzenecarbonitrile in 90% yield.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07425557B2uspto-grants-2008_09