Реакция #214459

ord-36911289438e4f93a2e3f19e78988076

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ФильтрацияIt is filtered
  2. 2
    Другоеthe filtrate evaporated
  3. 3
    workup.DISSOLUTIONthe residue dissolved in methylene chloride
  4. 4
    Промывкаthe solution washed with aqueous sodium carbonate
  5. 5
    Другоеdried
  6. 6
    Фильтрацияfiltered
  7. 7
    Другоеevaporated
  8. 8
    ДругоеThe residue is triturated with 50 ml of isopropanol

Методика

The mixture of 2.39 g of 4-amino-2-chloro-6,7-dimethoxyquinazoline, 2.64 g of 3-(4-piperidinyl)-3-azaspiro-[5,5]-undecan-2,4-dione, 2.1 g anhydrous sodium carbonate and 25 ml of dimethylformamide is stirred under nitrogen at 150° for 10 hours. It is filtered, the filtrate evaporated, the residue dissolved in methylene chloride, the solution washed with aqueous sodium carbonate, dried, filtered and evaporated. The residue is triturated with 50 ml of isopropanol, the remainder taken up in isopropanol and the mixture acidified with hydrogen chloride, to yield the 3-[2-(4-amino-6,7-dimethoxy-2-quinazolinyl)-4-piperidinyl]-3-azaspiro[5,5]undecan-2,4-dione monohydrochloride melting at 290° (dec.).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04255429uspto-grants-1981_03