반응 #8740

ord-7618583492454d46a32c9c9120713d00

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도Cool the reaction mixture
  2. 2
    농축concentrate
  3. 3
    기타to give a residue
  4. 4
    기타Purify the residue by column (silica) chromatography (ethyl acetate)
  5. 5
    농축Combine the appropriate fractions and concentrate

실험 절차

Combine a mixture (1 mmol total) of 3-[3-(3-bromo-propoxy)-phenyl]-thieno[2,3-d]isoxazole, 3-[3-(3-chloro-propoxy)-phenyl]-thieno[2,3-d]isoxazole with 2-fluorobenzylamine (0.63 g, 5.0 mmol), potassium carbonate (0.41 g, 3.0 mmol) and a mixture of acetonitrile:water (80:20) and heat (80° C.) for 30 hours. Cool the reaction mixture and concentrate to give a residue. Purify the residue by column (silica) chromatography (ethyl acetate). Combine the appropriate fractions and concentrate to give the title compound (0.36 g, 94% Yield) as an oil. Purity by LC/MS (APCI)=100% area, [M+H]+=383 g/mol.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091199B1uspto-grants-2006_08