HRID2120188

反应详情

EQUATION

反应方程式

HRID 2120188 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

To a solution of 8.27 g (0.04 mol) of the compound obtained in Example 4 in 39.4 ml of glacial acetic acid there are added, with sting, 25 ml of water, and to this solution there is slowly added a solution of 6.54 g of potassium cyanate in 10 ml of water. Once a white precipitate appears, the remaining potassium cyanate solution is added in one portion immediately. The mixture is warmed at 55° C., and stirred for 1 hour, then put aside at room temperature for 3 hours. 50 ml of water are added and the mixture is cooled to 5° C.; the separated solid is collected and dissolved in 10% sodium carbonate solution. Any insoluble material is filtered off and the filtrate is acidified with dilute sulphuric acid. The solid is collected and washed with water and dried, giving the title compound.

WORKUP

后处理

  1. waitput aside at room temperature for 3 hours
  2. temperaturethe mixture is cooled to 5° C.
  3. customthe separated solid is collected
  4. dissolutiondissolved in 10% sodium carbonate solution
  5. filtrationAny insoluble material is filtered off
  6. customThe solid is collected
  7. washwashed with water
  8. customdried