反応 #4620

反応方程式

benzylamine

sulphuric acid

5-(2-oxopropoxy)salicylamide

hydrogen

→

5-[2-(benzylamino)propoxy]salicylamide

溶媒

methanol

反応条件

後処理

1. 1
   ろ過The catalyst is filtered off
2. 2
   ろ過the solution is filtered again
3. 3
   濃縮concentrated by evaporation
4. 4
   その他The oil remaining crystallises from isopropanol
5. 5
   その他recrystallisation from isopropanol

実験手順

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°.

出典