HRID1174661

反应详情

EQUATION

反应方程式

HRID 1174661 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

A mixture of ethyl 4-hydroxycyclohexanecarboxylate (2.0 g, 12 mmol) and hydrazine (1.5 g, 46 mmol) in methanol (20 mL) was stirred at 55° C. for 4 h and then cooled to room temperature (about 25° C.). After cooling, the solvent and excess hydrazine were removed by distillation under reduced pressure to provide a residue. The residue was co-evaporated with methanol (2×), and was then dried under high vacuum to provide the crude product 4-hydroxycyclohexanecarbohydrazide, which was used in the next synthesis step without further purification. LCMS: (M+H)+=155.2.

WORKUP

后处理

  1. temperaturecooled to room temperature (about 25° C.)
  2. temperatureAfter cooling
  3. customthe solvent and excess hydrazine were removed by distillation under reduced pressure
  4. customto provide a residue
  5. customwas then dried under high vacuum