반응 #76685

ord-32fe8ca243f042448473b9ab80880ae9

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도to reflux for 1.5 hours
  2. 2
    기타The residue obtained
  3. 3
    workup.DISTILLATIONby distilling off the solvent under reduced pressure
  4. 4
    기타was purified by silica gel chromatography (hexane:ethyl acetate=2:1)
  5. 5
    기타The product obtained
  6. 6
    기타was crystallized from ethanol

실험 절차

4-cyano-5-ethoxymethyleneamino-3-aminoisoxazole (320 mg, 1.8 mmol) (see J. Org. Chem., 29, 2116 (1964)) and 2-aminoindan (710 mg, 5.3 mmol) in dry ethanol (3 ml) were heated to reflux for 1.5 hours. The residue obtained by distilling off the solvent under reduced pressure was purified by silica gel chromatography (hexane:ethyl acetate=2:1). The product obtained was crystallized from ethanol to obtain the title compound (270 mg, 0.38 mmol) having the following physical properties:

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06703421B1uspto-grants-2004_03