Reacción #214459

ord-36911289438e4f93a2e3f19e78988076

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    FiltraciónIt is filtered
  2. 2
    Otrothe filtrate evaporated
  3. 3
    workup.DISSOLUTIONthe residue dissolved in methylene chloride
  4. 4
    Lavadothe solution washed with aqueous sodium carbonate
  5. 5
    Otrodried
  6. 6
    Filtraciónfiltered
  7. 7
    Otroevaporated
  8. 8
    OtroThe residue is triturated with 50 ml of isopropanol

Procedimiento

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.).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US04255429uspto-grants-1981_03