반응 #92688

ord-9ff50a679ea74633aba031d749ee44b5

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도by heating
  2. 2
    온도to reflux overnight
  3. 3
    기타Under reduced pressure, the solvent was removed by filtration to around one third of the amount
  4. 4
    workup.ADDITIONa saturated aqueous sodium hydrogen carbonate solution and chloroform were then added
  5. 5
    기타a layer separation operation
  6. 6
    건조The organic layer was dried over anhydrous sodium sulfate
  7. 7
    기타the solvent was evaporated under reduced pressure
  8. 8
    기타The obtained residue was purified by silica gel column chromatography

실험 절차

To 350 mg of 8-[(2-fluorobenzyl)oxy]-2-methylimidazo[1,2-a]pyridine-6-carboxylic acid were added 18 ml of ethanol and 200 μl of sulfuric acid, followed by heating to reflux overnight. Under reduced pressure, the solvent was removed by filtration to around one third of the amount thereof, and a saturated aqueous sodium hydrogen carbonate solution and chloroform were then added thereto to carry out a layer separation operation. The organic layer was dried over anhydrous sodium sulfate and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain 330 mg of ethyl 8-[(2-fluorobenzyl)oxy]-2-methylimidazo[1,2-a]pyridine-6-carboxylate.

출처

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