تفاعل #4650

ord-fd0ebe5400be4198acdf81230619e204

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىhas been absorbed
  2. 2
    ترشيحThe catalyst is filtered off
  3. 3
    ترشيحthe mixture is again filtered
  4. 4
    تركيزconcentrated by evaporation
  5. 5
    أخرىbehind crystallises from isopropanol
  6. 6
    أخرىrecrystallisation from isopropanol

الإجراء التجريبي

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°.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04727067uspto-grants-1988_02