HRID42228

反应详情

EQUATION

反应方程式

HRID 42228 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
115 °C

PROCEDURE

实验过程

1H-Imidazole-4,5-dicarboxylic acid dimethyl ester (592 mg, 3.21 mmol) is combined with hydrazine (600 mg, 18.8 mmol) and MeOH (10 mL). The reaction mixture is heated to 115° C. for 30 min. Cool and filter off the resulting precipitate. Wash with additional water. Combine the precipitate with hydrazine (1.38 mL) and reflux for 4 h. Pour the reaction mixture into ice water and adjust the to pH 2 with HCl (12 N). The new precipitate is isolated by filtration to afford the title product (293 mg, 60%)

WORKUP

后处理

  1. temperatureCool
  2. filtrationfilter off the resulting precipitate
  3. washWash with additional water
  4. temperaturereflux for 4 h
  5. additionPour the reaction mixture into ice water
  6. customThe new precipitate is isolated by filtration