Реакция #4660

ord-961546021a8f448e97a2a1b9f8a02a55

Растворители

Условия реакции

Температура
60°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.WAITleft
  2. 2
    Температураto cool
  3. 3
    workup.WAITleft
  4. 4
    Температураto cool
  5. 5
    Другоеthe precipitate formed
  6. 6
    Фильтрацияis filtered off
  7. 7
    Промывкаwashed with water
  8. 8
    Другоеrecrystallized from a dimethylformamide/water mixture (1:1)

Методика

A mixture of 3.2 g (0.011 mol) of ethyl 6-fluoro-7-(pyrrol-1-yl)-4-hydroxyquinoline-3-carboxylate and 4 g (2.5×0.011 mol) of potassium carbonate in 20 ml of dimethylformamide is heated for 30 minutes at 60° C. and left to cool, 7 g (5×0.011 mol) of bromofluoroethane are added, the mixture is kept for 7 hours at 80° C., left to cool and poured into a water/ice mixture, and the precipitate formed is filtered off, washed with water and recrystallized from a dimethylformamide/water mixture (1:1) to give 2.35 g of a solid melting at 231°-234° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04727080uspto-grants-1988_02