Реакция #93524

ord-8845ad20acfe403ba0366227d1ec6e70

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураHeat
  2. 2
    Другоеthe reaction by thin-layer chromatography on silica gel (acetonitrile: ammonium hydroxide, 90:10)
  3. 3
    ДругоеAt the completion of the reaction
  4. 4
    Другоеtriturate the
  5. 5
    Температураcooled resultant material with petroleum ether
  6. 6
    ДругоеRecrystallize the material from 25 ml hot methyl ethyl ketone
  7. 7
    Фильтрацияwith hot filtration
  8. 8
    Температураchill

Методика

Heat a mixture of 6.23 g (0.017 mole) 4-methylbenzenesulfonic acid 4-(4-acetylaminophenyl)butyl ester and 2.9 g (0.017 mole) 1-heptyl-1H-imidazole to 80° C., for 5 hours, following the reaction by thin-layer chromatography on silica gel (acetonitrile: ammonium hydroxide, 90:10). At the completion of the reaction, triturate the cooled resultant material with petroleum ether. Recrystallize the material from 25 ml hot methyl ethyl ketone with hot filtration, chill and seed to obtain the title compound.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04613609uspto-grants-1986_09