反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe suspension obtained
- customclose to 50° C under a hydrogen atmosphere (100 kPa)
- temperatureAfter cooling
- customthe catalyst is separated off by filtration
- concentrationthe solution is concentrated to dryness under reduced pressure (2.7 kPa) at 35° C
- customThe residue obtained
- customThe insoluble product formed
- customis separated off by filtration
- customair-dried
- customrecrystallization from ethanol