반응 #60789

ord-788ae941d6bc4b03b8f7827949398947

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted with EtOAc (3×20 mL)
  2. 2
    세척further washed with water (10 mL), aqueous sodium hydrogen carbonate solution (10 mL)
  3. 3
    건조Organics were dried (MgSO4)
  4. 4
    기타evaporated
  5. 5
    기타to give a pale gum

실험 절차

A suspension of 1-methyl-4-phenyl-1H-imidazole-5-carbonyl chloride (intermediate 4) (0.80 g) in anhydrous NMP (2 mL) was added to aminomalononitrile p-toluenesulfonate (0.92 g) in anhydrous NMP (10 mL). The resultant mixture was stirred for 24 hours. The mixture was poured into water (10 mL), extracted with EtOAc (3×20 mL), organics combined and further washed with water (10 mL), aqueous sodium hydrogen carbonate solution (10 mL) then brine (10 mL). Organics were dried (MgSO4) and evaporated to give a pale gum. Trituration with isohexane (5 mL) gave the title compound as a white solid (650 mg, 68%);

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07427616B2uspto-grants-2008_09