반응 #92687

ord-2d92678427e44e14afb990b87d1e5427

용매

반응 조건

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

후처리

  1. 1
    workup.STIRRINGby stirring at 80° C. for 4 hours
  2. 2
    기타the solvent was evaporated under reduced pressure
  3. 3
    추출by extracting with ethyl acetate
  4. 4
    세척washing with saturated brine
  5. 5
    건조After drying over anhydrous magnesium sulfate
  6. 6
    여과filtering
  7. 7
    기타the solvent was evaporated under reduced pressure
  8. 8
    기타The obtained residue was purified by silica gel column chromatography

실험 절차

To a suspension of 2.15 g of methyl 6-amino-5-[(2-fluorobenzyl)oxy]nicotinate in 43 ml of ethanol was added 1.09 ml of bromoacetone, followed by stirring at 80° C. for 4 hours. To the reaction mixture was added 1.09 ml of bromoacetone, followed by stirring at 80° C. for 4 hours. To the reaction mixture was added a saturated aqueous sodium hydrogen carbonate solution, and the solvent was evaporated under reduced pressure, followed by extracting with ethyl acetate and washing with saturated brine. After drying over anhydrous magnesium sulfate and then filtering, the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain 1.39 g of methyl 8-[(2-fluorobenzyl)oxy]-2-methylimidazo[1,2-a]pyridine-6-carboxylate.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09447090B2uspto-grants-2016_09