Реакция #94446

ord-b80ae327a1504a2aa6409de3523f995e

Реагенты

Нет

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураheated together in a nitrogen atmosphere
  2. 2
    ТемператураThe reaction mixture is cooled
  3. 3
    Другоеsubsequently chromatographed on silica gel with an ethyl acetate/hexane mixture as the eluant
  4. 4
    Другоеcrystallised from ether

Методика

12.7 g (0.1 mole) of 2-ethoxy-3,4,5,6-tetrahydropyridine and 24.4 g (0.15 mole) of 1-phenyl-1,3-butanedione are mixed and heated together in a nitrogen atmosphere, with stirring, for 32 hours in an oil bath at 100°. The reaction mixture is cooled, and subsequently chromatographed on silica gel with an ethyl acetate/hexane mixture as the eluant. The main fractions are combined and crystallised from ether to obtain 1-phenyl-2-(2-piperidinylidene)-1,3-butanedione in the form of yellow crystals, m.p. 80°-81°.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04130652uspto-grants-1978_12