تفاعل #214459

ord-36911289438e4f93a2e3f19e78988076

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحIt is filtered
  2. 2
    أخرىthe filtrate evaporated
  3. 3
    workup.DISSOLUTIONthe residue dissolved in methylene chloride
  4. 4
    غسيلthe solution washed with aqueous sodium carbonate
  5. 5
    أخرىdried
  6. 6
    ترشيحfiltered
  7. 7
    أخرىevaporated
  8. 8
    أخرىThe residue is triturated with 50 ml of isopropanol

الإجراء التجريبي

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.).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04255429uspto-grants-1981_03