تفاعل #214458

معادلة التفاعل

4-amino-2-chloro-6,7,8-trimethoxyquinazoline

8-(4-piperidinyl)-8-azaspiro-[4,5]decan-7,9-dione

sodium carbonate

→

8-[1-(4-amino-6,7,8-trimethoxy-2-quinazolinyl)-4-piperidinyl]-8-azaspiro[4,5]decan-7,9dione monohydrochloride

المذيبات

dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   ترشيحis filtered
2. 2
   أخرىthe filtrate evaporated
3. 3
   workup.DISSOLUTIONthe residue dissolved in ethyl acetate
4. 4
   غسيلthe solution washed with aqueous sodium bicarbonate and water
5. 5
   أخرىIt is dried
6. 6
   أخرىevaporated
7. 7
   workup.DISSOLUTIONthe residue dissolved in 75 ml of ethyl acetate
8. 8
   أخرىto crystallize
9. 9
   workup.DISSOLUTIONThe crystals are dissolved in 50 ml of hot isopropanol
10. 10
    ترشيحthe precipitate filtered off

الإجراء التجريبي

The mixture of 5.39 g of 4-amino-2-chloro-6,7,8-trimethoxyquinazoline, 5.25 g of 8-(4-piperidinyl)-8-azaspiro-[4,5]decan-7,9-dione, 4.24 g of anhydrouus sodium carbonate and 75 ml of dimethylformamide is stirred at 150° for 8 hours. After cooling to room temperature it is filtered, the filtrate evaporated, the residue dissolved in ethyl acetate and the solution washed with aqueous sodium bicarbonate and water. It is dried, evaporated, the residue dissolved in 75 ml of ethyl acetate and allowed to crystallize. The crystals are dissolved in 50 ml of hot isopropanol and the solution acidified with hydrogen chloride to pH=1 and the precipitate filtered off, to yield the 8-[1-(4-amino-6,7,8-trimethoxy-2-quinazolinyl)-4-piperidinyl]-8-azaspiro[4,5]decan-7,9dione monohydrochloride melting at 225°-227°.

المصدر