تفاعل #40717

ord-7a8b9422f4634db6947a7b29d86ba228

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىDuring the reaction
  2. 2
    أخرىAfter that, EtOH was evaporated off
  3. 3
    أخرىthe resulting oil was dried in vacuum
  4. 4
    أخرىTrituration with ether (15 mL) gave light brown solids, which
  5. 5
    أخرىwere removed by filtration
  6. 6
    غسيلwashed with ether
  7. 7
    workup.DISSOLUTIONThe solids then re-dissolved in CHCl3
  8. 8
    ترشيحfiltered
  9. 9
    أخرىAfter evaporation of the solvent
  10. 10
    أخرىlight brown solids were obtained (0.35 g, 50%)

الإجراء التجريبي

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%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07728016B2uspto-grants-2010_06