تفاعل #214462

ord-faf9295f48a842a48eb8a5dd0b9cfae3

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 bicarbonate
  5. 5
    أخرىThe organic layer is separated
  6. 6
    أخرىdried
  7. 7
    أخرىevaporated
  8. 8
    درجة الحرارةin refluxing isopropanol
  9. 9
    أخرىThe precipitate formed
  10. 10
    ترشيحis filtered off
  11. 11
    أخرىtriturated with warm ethanol

الإجراء التجريبي

The mixture of 5.39 g of 4-amino-2-chloro-6,7,8-trimethoxy-quinazoline, 4.32 g of 2-(4-piperidinyl)-isoindolin-1-one, 4.24 g of anhydrous sodium carbonate and 75 ml of dimethylformamide is stirred under nitrogen at 125°-130° for 16 hours. It is filtered, the filtrate evaporated, the residue dissolved in methylene chloride and the solution washed with aqueous sodium bicarbonate. The organic layer is separated, dried, and evaporated. The residue is suspended in refluxing isopropanol and acidified with hydrogen chloride to pH=1. The precipitate formed is filtered off and triturated with warm ethanol to yield the 2-[1-(4-amino-6,7,8-trimethoxy-2-quinazolinyl)-4-piperidinyl]-isoindolin-1-one monohydrochloride melting at 234° (dec.).

المصدر

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