반응 #214459

반응 방정식

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

3-(4-piperidinyl)-3-azaspiro-[5,5]-undecan-2,4-dione

sodium carbonate

→

3-[2-(4-amino-6,7-dimethoxy-2-quinazolinyl)-4-piperidinyl]-3-azaspiro[5,5]undecan-2,4-dione monohydrochloride

용매

dimethylformamide

반응 조건

후처리

1. 1
   여과It is filtered
2. 2
   기타the filtrate evaporated
3. 3
   workup.DISSOLUTIONthe residue dissolved in methylene chloride
4. 4
   세척the solution washed with aqueous sodium carbonate
5. 5
   기타dried
6. 6
   여과filtered
7. 7
   기타evaporated
8. 8
   기타The residue is triturated with 50 ml of isopropanol

실험 절차

The mixture of 2.39 g of 4-amino-2-chloro-6,7-dimethoxyquinazoline, 2.64 g of 3-(4-piperidinyl)-3-azaspiro-[5,5]-undecan-2,4-dione, 2.1 g anhydrous sodium carbonate and 25 ml of dimethylformamide is stirred under nitrogen at 150° for 10 hours. It is filtered, the filtrate evaporated, the residue dissolved in methylene chloride, the solution washed with aqueous sodium carbonate, dried, filtered and evaporated. The residue is triturated with 50 ml of isopropanol, the remainder taken up in isopropanol and the mixture acidified with hydrogen chloride, to yield the 3-[2-(4-amino-6,7-dimethoxy-2-quinazolinyl)-4-piperidinyl]-3-azaspiro[5,5]undecan-2,4-dione monohydrochloride melting at 290° (dec.).

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