反応 #8455

ord-47a419c279bd4298997bf49bc82a7f5a

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the solvent evaporated in vacuo
  2. 2
    workup.DISSOLUTIONThe residue was dissolved in dichloromethane (75 mL)
  3. 3
    洗浄washed with saturated sodium bicarbonate solution (2×75 mL), brine (75 mL)
  4. 4
    乾燥dried over magnesium sulfate
  5. 5
    ろ過filtered
  6. 6
    その他evaporated
  7. 7
    その他The residue was purified via silica gel chromatography (ethyl acetate/hexane)

実験手順

A solution of the product of Step B (2.6 g) and 2-amino-4-picoline (0.96 g) in ethanol (10 mL) was heated at 73° C. for 2 hours. The reaction mixture was cooled to ambient temperature and the solvent evaporated in vacuo. The residue was dissolved in dichloromethane (75 mL), washed with saturated sodium bicarbonate solution (2×75 mL), brine (75 mL), dried over magnesium sulfate, filtered and evaporated. The residue was purified via silica gel chromatography (ethyl acetate/hexane) to give the title compound (1.3 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07087757B2uspto-grants-2006_08