反応 #214458

反応方程式

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

溶媒

dimethylformamide

反応条件

後処理

1. 1
   ろ過is filtered
2. 2
   その他the filtrate evaporated
3. 3
   workup.DISSOLUTIONthe residue dissolved in ethyl acetate
4. 4
   洗浄the solution washed with aqueous sodium bicarbonate and water
5. 5
   その他It is dried
6. 6
   その他evaporated
7. 7
   workup.DISSOLUTIONthe residue dissolved in 75 ml of ethyl acetate
8. 8
   その他to crystallize
9. 9
   workup.DISSOLUTIONThe crystals are dissolved in 50 ml of hot isopropanol
10. 10
    ろ過the precipitate filtered off

実験手順

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°.

出典