Реакция #76685

ord-32fe8ca243f042448473b9ab80880ae9

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

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

Методика

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:

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06703421B1uspto-grants-2004_03