تفاعل #214462
ord-faf9295f48a842a48eb8a5dd0b9cfae3
معادلة التفاعل
المتفاعلات
الكواشف
المذيبات
ظروف التفاعل
المعالجة
- 1ترشيحIt is filtered
- 2أخرىthe filtrate evaporated
- 3workup.DISSOLUTIONthe residue dissolved in methylene chloride
- 4غسيلthe solution washed with aqueous sodium bicarbonate
- 5أخرىThe organic layer is separated
- 6أخرىdried
- 7أخرىevaporated
- 8درجة الحرارةin refluxing isopropanol
- 9أخرىThe precipitate formed
- 10ترشيحis filtered off
- 11أخرىtriturated 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.).