반응 #92742

ord-7e976c4e9c9f48098fa2f6a15b511287

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooling
  2. 2
    온도cooling
  3. 3
    기타a layer separation operation
  4. 4
    건조The organic layer was dried over anhydrous sodium sulfate
  5. 5
    기타the solvent was evaporated under reduced pressure
  6. 6
    기타The obtained residue was purified by silica gel column chromatography

실험 절차

To a suspension of 307 mg of 8-(cyclohexylmethoxy)-2-methyl-N-[(3S)-piperidin-3-yl]imidazo[1,2-a]pyridine-3-carboxamide dihydrochloride, 335 mg of potassium carbonate, 5 ml of acetonitrile, and 5 ml of DMF was added 92 μl of bromoethyl acetate under ice-cooling, followed by stirring for 3 hours under ice-cooling. To the reaction mixture were added water and chloroform 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 299 mg of ethyl[(3S)-3-({[8-(cyclohexylmethoxy)-2-methylimidazo[1,2-a]pyridin-3-yl]carbonyl}amino)piperidin-1-yl]acetate.

출처

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