HRID4554

反应详情

EQUATION

反应方程式

HRID 4554 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

55 g of benzylamine and 1.25 g of conc. sulfuric acid are added to a solution of 104.5 g of 5-(2-oxo-propoxy)salicylamide in 1000 ml of methanol, and the mixture is hydrogenated, in the presence of 3.0 g of a Pt/C catalyst under normal conditions until 1 equivalent of hydrogen has been absorbed. The catalyst is filtered off, and the solution is then stirred up with about 10 g of pulverised calcium carbonate; the mixture is again filtered, and concentrated by evaporation. The oil remaining behind crystallises from isopropanol. Repeated recrystallisation from isopropanol yields 5-[2-(benzylamino)-propoxy]-salicylamide, m.p. 102°-104°.

WORKUP

后处理

  1. customhas been absorbed
  2. filtrationThe catalyst is filtered off
  3. filtrationthe mixture is again filtered
  4. concentrationconcentrated by evaporation
  5. custombehind crystallises from isopropanol
  6. customrecrystallisation from isopropanol