반응 #76682

ord-024ce929433f44509d6cf287f724db6b

반응 조건

온도
130°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was heated
  2. 2
    온도The reaction mixture was cooled
  3. 3
    온도which was further heated
  4. 4
    온도to reflux at 130° C. for 2 hours
  5. 5
    기타The residue obtained
  6. 6
    workup.DISTILLATIONby distilling off the solvent under reduced pressure
  7. 7
    기타was purified by silica gel chromatography (hexane:ethyl acetate=2:1)

실험 절차

A mixture of 2-amino-3-cyanofuran (270 mg, 2.5 mmol), triethyl orthoformate (1.5 ml, 9.0 mmol), and acetic anhydride (0.18 ml, 1.9 mmol) was heated to reflux at 130° C. for 2 hours. The reaction mixture was cooled, and 2-aminoindan (670 mg, 5.0 mmol), sodium acetate (640 mg, 7.8 mmol), and acetic acid (1.1 ml, 19 mmol) were added, which was further heated to reflux at 130° C. for 2 hours. The residue obtained by distilling off the solvent under reduced pressure was purified by silica gel chromatography (hexane:ethyl acetate=2:1) to obtain the title compound (44 mg, 0.18 mmol) having the following physical properties:

출처

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