HRID514689

反应详情

EQUATION

反应方程式

HRID 514689 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

Under the nitrogen atmosphere, 5.0 g of 5-hydroxy-1H-imidazole-4-carboxamide hydrochloric acid salt dihydrate prepared according to the method of Comparative Example 4 (1) was added to 60 mL of 0.45 mol/L hydrochloric acid and dissolved therein by heating to 40 to 50° C. To the solution, 3.9 mL of 25% ammonia water was added dropwise over 10 minutes. pH of the reaction mixture was 6.6. After the dropwise addition was completed, the reaction solution was cooled to room temperature and stirred for 1 hour. The crystal was collected by filtration and then washed with a mixture liquid containing 5 mL of acetone and 10 mL of water followed by 15 mL of acetone to give 0.54 g of 5-hydroxy-1H-imidazole-4-carboxamide.3/4 hydrate as a blue crystal.

WORKUP

后处理

  1. dissolutiondissolved
  2. additionAfter the dropwise addition
  3. temperaturethe reaction solution was cooled to room temperature
  4. filtrationThe crystal was collected by filtration
  5. washwashed with a mixture liquid
  6. additioncontaining 5 mL of acetone and 10 mL of water