반응 #92678

ord-d2d55b23c17241fd92a6743415c415e4

반응 조건

온도
110°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타After leaving
  2. 2
    온도to be cooled at room temperature
  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 solution of 1.38 g of 3-(cyclohexylmethoxy)-5-methylpyridin-2-amine in 24 ml of toluene were added 1.21 ml of ethyl 2-chloro-3-oxobutanoate and 1.23 ml of triethylamine, followed by stirring at 110° C. for 3 days. After leaving to be cooled at room temperature, water and diisopropyl ether were 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 1.52 g of ethyl 8-(cyclohexylmethoxy)-2,6-dimethylimidazo[1,2-a]pyridine-3-carboxylate.

출처

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