反応 #214455

反応方程式

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

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 ethyl acetate
4. 4
   洗浄the solution washed with aqueous sodium carbonate and water
5. 5
   その他It is dried
6. 6
   その他evaporated
7. 7
   その他the residue triturated with isopropanol
8. 8
   ろ過filtered off
9. 9
   ろ過the precipitate filtered off
10. 10
    その他triturated with 175 ml of boiling methanol

実験手順

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.

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