HRID514681

反应详情

EQUATION

反应方程式

HRID 514681 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
82 °C

PROCEDURE

实验过程

Under the nitrogen atmosphere, 30 g of 2-aminomalonamide and 115 mg of oxalic acid were added to 600 mL of 2-propanol. After heating to 82° C., 106 mL of triethyl orthoformate was added dropwise to the mixture over 10 minutes. Subsequently, the reaction mixture was stirred for 7 hours and 30 minutes at 84° C. Subsequently, after cooling to 57° C., the reaction mixture was added with 30 mL of water followed by 24 mL of conc. hydrochloric acid. After cooling the reaction mixture to 5° C., the crystal was collected by filtration and then washed with 120 mL of acetone to give 49 g of 5-hydroxy-1H-imidazole-4-carboxamide hydrochloric acid salt dihydrate as a pale yellow crystal.

WORKUP

后处理

  1. temperatureSubsequently, after cooling to 57° C.
  2. temperatureAfter cooling the reaction mixture to 5° C.
  3. filtrationthe crystal was collected by filtration
  4. washwashed with 120 mL of acetone