반응 #214455

반응 방정식

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

용매

dimethylformamide

반응 조건

후처리

1. 1
   여과It is filtered
2. 2
   기타the filtrate evaporated
3. 3
   workup.DISSOLUTIONthe residue dissolved in ethyl acetate
4. 4
   세척the solution washed with aqueous sodium carbonate and water
5. 5
   기타It is dried
6. 6
   기타evaporated
7. 7
   기타the residue triturated with isopropanol
8. 8
   여과filtered off
9. 9
   여과the precipitate filtered off
10. 10
    기타triturated with 175 ml of boiling methanol

실험 절차

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.

출처