반응 #214462

반응 방정식

4-amino-2-chloro-6,7,8-trimethoxy-quinazoline

2-(4-piperidinyl)-isoindolin-1-one

sodium carbonate

→

2-[1-(4-amino-6,7,8-trimethoxy-2-quinazolinyl)-4-piperidinyl]-isoindolin-1-one 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 bicarbonate
5. 5
   기타The organic layer is separated
6. 6
   기타dried
7. 7
   기타evaporated
8. 8
   온도in refluxing isopropanol
9. 9
   기타The precipitate formed
10. 10
    여과is filtered off
11. 11
    기타triturated with warm ethanol

실험 절차

The mixture of 5.39 g of 4-amino-2-chloro-6,7,8-trimethoxy-quinazoline, 4.32 g of 2-(4-piperidinyl)-isoindolin-1-one, 4.24 g of anhydrous sodium carbonate and 75 ml of dimethylformamide is stirred under nitrogen at 125°-130° for 16 hours. It is filtered, the filtrate evaporated, the residue dissolved in methylene chloride and the solution washed with aqueous sodium bicarbonate. The organic layer is separated, dried, and evaporated. The residue is suspended in refluxing isopropanol and acidified with hydrogen chloride to pH=1. The precipitate formed is filtered off and triturated with warm ethanol to yield the 2-[1-(4-amino-6,7,8-trimethoxy-2-quinazolinyl)-4-piperidinyl]-isoindolin-1-one monohydrochloride melting at 234° (dec.).

출처