HRID591221

反应详情

EQUATION

反应方程式

HRID 591221 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

To a stirring solution of NaOEt prepared from sodium (FLUKA, 9.19 g, 400 mmol) and ethanol (350 mL) was added aminoguanidine hydrochloride (ALDRICH, 44.2 g, 400 mmol). The reaction mixture was heated at 50° C. for 30 min. Then, the mixture was filtered to remove NaCl, and ethyl 3-oxobutanoate (ALDRICH, 25.3 mL, 200 mmol) was added to the filtrate. The reaction mixture was heated under reflux for 5 h and, then, stirred at room temperature overnight. The precipitate obtained was filtered and dried under vacuum to afford Intermediate 1 as a pale pink solid.

WORKUP

后处理

  1. filtrationThen, the mixture was filtered
  2. additionwas added to the filtrate
  3. temperatureThe reaction mixture was heated
  4. temperatureunder reflux for 5 h
  5. customThe precipitate obtained
  6. filtrationwas filtered
  7. customdried under vacuum