HRID2289183

反应详情

EQUATION

反应方程式

HRID 2289183 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

Cyanoacetylurea (116.1 g) was suspended in N,N-dimethylformamide (219.3 ml), and acetone (73.1 ml), acetic acid (10.8 ml) and ammonium acetate (6.93 g) were added. This suspension was subjected to catalytic hydrogenation in the presence of 10% palladium carbon (2.33 g, 50% wet product) under hydrogen pressure at 10 kg/cm2 and at 25° C. for 4 hours. The reaction mixture was heated to 70° C., and the catalyst was filtered off. Water (745 ml) was added to the filtrate to allow precipitation of crystals. The crystals were collected by filtration to give crystals of N-(2-cyano-3-methylbutanoyl)urea (yield 134.5 g).

WORKUP

后处理

  1. filtrationthe catalyst was filtered off
  2. additionWater (745 ml) was added to the filtrate
  3. customprecipitation of crystals
  4. filtrationThe crystals were collected by filtration