Реакция #1379890

ord-e796985f790a46e48b1f769398221cab

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураat reflux for 48 h
  2. 2
    Температураto cool to ambient,
  3. 3
    Экстракцияthe filtrate extracted with diethyl ether (3×100 ml)
  4. 4
    ДругоеThe precipitate which formed
  5. 5
    Фильтрацияwas collected by filtration
  6. 6
    Промывкаwashed first with water (200 ml)
  7. 7
    Сушкаwith acetone (200 ml) before being dried

Методика

A mixture of 5-aminoquinoline (9.9 g, 0.069 mol) and crotonic acid (8.9 g, 0.103 mol) in toluene (35 ml) was stirred at reflux for 48 h. The reaction mixture was allowed to cool to ambient, added to water (500 ml) and the pH adjusted to 9 to 10 by the addition of 2N sodium hydroxide. The reaction mixture was screened and the filtrate extracted with diethyl ether (3×100 ml). The pH of the aqueous layer was first adjusted to pH2 with concentrated HCl and then to pH7 with calcium hydroxide. The precipitate which formed was collected by filtration, washed first with water (200 ml) and then with acetone (200 ml) before being dried to give 8.1 g of a cream solid.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07238228B2uspto-grants-2007_07