반응 #40717

ord-7a8b9422f4634db6947a7b29d86ba228

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타During the reaction
  2. 2
    기타After that, EtOH was evaporated off
  3. 3
    기타the resulting oil was dried in vacuum
  4. 4
    기타Trituration with ether (15 mL) gave light brown solids, which
  5. 5
    기타were removed by filtration
  6. 6
    세척washed with ether
  7. 7
    workup.DISSOLUTIONThe solids then re-dissolved in CHCl3
  8. 8
    여과filtered
  9. 9
    기타After evaporation of the solvent
  10. 10
    기타light brown solids were obtained (0.35 g, 50%)

실험 절차

1-Azido-5-chloro-2,4-dimethoxy-benzene (0.4 g, 1.9 mmol), 3-(4-Fluoro-phenyl)-3-oxo-propionic acid methyl ester (0.42 g, 2.2 mmol) and sodium ethoxide in EtOH (70 mg of sodium in 15 mL EtOH) were refluxed for 3 hours. During the reaction, the solution turned brown from dark green. After that, EtOH was evaporated off and the resulting oil was dried in vacuum. Trituration with ether (15 mL) gave light brown solids, which were removed by filtration and washed with ether. The solids then re-dissolved in CHCl3 and filtered. After evaporation of the solvent, light brown solids were obtained (0.35 g, 50%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07728016B2uspto-grants-2010_06