تفاعل #214455

معادلة التفاعل

4-amino-2-chloro-6,7-dimethoxyquinazoline

4,4-dimethyl-1-(4-piperidinyl)-piperidin-2,6-dione

sodium carbonate

→

1-[1-(4-amino-6,7-dimethoxy-2-quinazolinyl)-4-piperidinyl]-4,4-dimethyl-piperidin-2,6-dione monohydrochloride

المذيبات

dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   ترشيحIt is filtered
2. 2
   أخرىthe filtrate evaporated
3. 3
   workup.DISSOLUTIONthe residue dissolved in ethyl acetate
4. 4
   غسيلthe solution washed with aqueous sodium carbonate and water
5. 5
   أخرىIt is dried
6. 6
   أخرىevaporated
7. 7
   أخرىthe residue triturated with isopropanol
8. 8
   ترشيحfiltered off
9. 9
   ترشيحthe precipitate filtered off
10. 10
    أخرىtriturated with 175 ml of boiling methanol

الإجراء التجريبي

The mixture of 4.79 g of 4-amino-2-chloro-6,7-dimethoxyquinazoline, 4.49 g of 4,4-dimethyl-1-(4-piperidinyl)-piperidin-2,6-dione, 4.24 g of anhydrous sodium carbonate and 75 ml of dimethylformamide is stirred at 150° under nitrogen for 6 hours. It is filtered, the filtrate evaporated, the residue dissolved in ethyl acetate and the solution washed with aqueous sodium carbonate and water. It is dried, evaporated, the residue triturated with isopropanol, filtered off and discarded. The filtrate is made strongly acidic with hydrogen chloride, the precipitate filtered off and triturated with 175 ml of boiling methanol, to yield the 1-[1-(4-amino-6,7-dimethoxy-2-quinazolinyl)-4-piperidinyl]-4,4-dimethyl-piperidin-2,6-dione monohydrochloride, melting at 279°-280° with decomposition.

المصدر