反应 #4620

ord-93a5ea0a4f844f3b992c9c05b03c834a

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤The catalyst is filtered off
  2. 2
    过滤the solution is filtered again
  3. 3
    浓缩concentrated by evaporation
  4. 4
    其他The oil remaining crystallises from isopropanol
  5. 5
    其他recrystallisation from isopropanol

实验过程

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°.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04727067uspto-grants-1988_02