反応 #214459

反応方程式

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

溶媒

dimethylformamide

反応条件

後処理

1. 1
   ろ過It is filtered
2. 2
   その他the filtrate evaporated
3. 3
   workup.DISSOLUTIONthe residue dissolved in methylene chloride
4. 4
   洗浄the solution washed with aqueous sodium carbonate
5. 5
   その他dried
6. 6
   ろ過filtered
7. 7
   その他evaporated
8. 8
   その他The residue is triturated with 50 ml of isopropanol

実験手順

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.).

出典