Реакция #321866

ord-9a09b32cb1054981bb27fa8a71fade94

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe crude reaction product
  2. 2
    Другоеwas purified on 200 g of aluminium oxide (activity grade II)
  3. 3
    Другоеto recrystallization
  4. 4
    workup.ADDITIONa 1:1 mixture of toluene and acetone
  5. 5
    Промывкаthe product was eluted
  6. 6
    Другоеafter recrystallization from 5 ml of acetonitrile

Методика

4.57 g of 4,7-dichloroquinoline, 7.5 g of 2-methyl-2-(piperidin-1-yl)-propylamine and 0.75 g of phenol were reacted at 180° C. for 16 hours. The crude reaction product, isolated as in the preceeding Example, was purified on 200 g of aluminium oxide (activity grade II) prior to recrystallization; a 1:1 mixture of toluene and acetone was used as the eluent. After a fore-run, which contained unreacted 4,7-dichloroquinoline, the product was eluted and, after recrystallization from 5 ml of acetonitrile, yielded 0.8 g of colourless crystals, m.p.: 143°-147° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05596002uspto-grants-1997_01