반응 #4620

반응 방정식

benzylamine

sulphuric acid

5-(2-oxopropoxy)salicylamide

hydrogen

→

5-[2-(benzylamino)propoxy]salicylamide

용매

methanol

반응 조건

후처리

1. 1
   여과The catalyst is filtered off
2. 2
   여과the solution is filtered again
3. 3
   농축concentrated by evaporation
4. 4
   기타The oil remaining crystallises from isopropanol
5. 5
   기타recrystallisation from isopropanol

실험 절차

55 g of benzylamine and 1.25 g of concentrated sulphuric acid are added to a solution of 104.5 g of 5-(2-oxopropoxy)salicylamide in 100 ml of methanol and hydrogenated in the presence of 3.0 g of Pt/C-catalyst at room temperature and atmospheric pressure until 1 equivalent of hydrogen has been absorbed. The catalyst is filtered off, approximately 10 g of powdered calcium carbonate are stirred into the solution and the solution is filtered again and concentrated by evaporation. The oil remaining crystallises from isopropanol. Repeated recrystallisation from isopropanol yields 5-[2-(benzylamino)propoxy]salicylamide having a melting point of 102°-104°.

출처