반응 #4682

ord-e8342923f9524540becdf8521b43cb93

용매

반응 조건

온도
-5°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The solvent is then evaporated
  2. 2
    workup.ADDITION15 ml of boiling methanol are added to the residue

실험 절차

20 g (0.07 moles) of 2-(4-acetylaminobenzoyloxy)ethyl acetylacetate, 8.41 (0.07 moles) of ethyl 3-aminocrotonate and 9.84 g (0.07 moles) of 3-nitrobenzaldehyde are heated under reflux in 65 ml of ethanol for 8 hours. The solvent is then evaporated, 15 ml of boiling methanol are added to the residue, the solution is discoloured with activated charcoal and cooled to -5° C. to obtain 2-(4-acetylaminobenzoyloxy)ethyl 2,6-dimethyl-5-ethoxycarbonyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3-carboxylate with half a molecule of ethanol as yellow crystals melting--after recrystallisation in ehtanol--at 157°-162° C. The yield is 46% of the theoretical yield.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04727066uspto-grants-1988_02