HRID1769713

反应详情

EQUATION

反应方程式

HRID 1769713 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

0.3 g of 5% palladium-on-charcoal is added to a solution of 1.8 g of N-methyl-2-{2-[3-(3-nitrophenyl)ureido]-N-phenylacetamido}-N-phenylacetamide in 100 cm3 of ethanol. The suspension obtained is stirred for 2 hours at a temperature close to 50° C under a hydrogen atmosphere (100 kPa). After cooling, the catalyst is separated off by filtration and the solution is concentrated to dryness under reduced pressure (2.7 kPa) at 35° C. The residue obtained is dissolved in 60 cm3 of an acetonitrile/diisopropyl ether mixture (20/80 by volume) and 5 cm3 of a 3.5N solution of hydrochloric acid in diisopropyl ether are added. The insoluble product formed is separated off by filtration, air-dried and recrystallization from ethanol. 0.9 g of 2-{2-[3-(3-aminophenyl)ureido]-N-phenylacetamido}-N-methyl-N-phenylacetamide hydrochloride melting at 220° C is thus obtained.

WORKUP

后处理

  1. customThe suspension obtained
  2. customclose to 50° C under a hydrogen atmosphere (100 kPa)
  3. temperatureAfter cooling
  4. customthe catalyst is separated off by filtration
  5. concentrationthe solution is concentrated to dryness under reduced pressure (2.7 kPa) at 35° C
  6. customThe residue obtained
  7. customThe insoluble product formed
  8. customis separated off by filtration
  9. customair-dried
  10. customrecrystallization from ethanol