HRID539627

反应详情

EQUATION

反应方程式

HRID 539627 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirring solution of 6-phenyl-piperidin-2-one (0.35 g, 2 mmol) in methylene chloride (1 mL) at 0° C. under nitrogen atmosphere was added methyl triflate (0.23 mL, 2 mmol). The reaction mixture was stirred at room temperature for three hours, then added to a stirring 0°C solution of anhydrous hydrazine (0.5 mL) in methanol (1 mL). The mixture was stirred for 3.5 hours at room temperature, then poured into a 1:1 mixture of methylene chloride and diethyl ether. The mixture was washed with 1.5M aqueous sodium carbonate, dried over anhydrous potassium carbonate, filtered, and concentrated under reduced pressure to give 0.34 g (90%) of [6-phenyl-piperidin-(2Z)-ylidene]-hydrazine as a colorless oil.

WORKUP

后处理

  1. stirringThe mixture was stirred for 3.5 hours at room temperature
  2. washThe mixture was washed with 1.5M aqueous sodium carbonate
  3. dry with materialdried over anhydrous potassium carbonate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure