HRID465049

反应详情

EQUATION

反应方程式

HRID 465049 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

With stirring and external cooling with ice, a solution of 2-(chloromethyl)pyridine hydrochloride (100 g, 0.61 mol) in 95% ethanol (600 ml) is added dropwise to pyrrolidine (500 ml, 426 g, 5.99 mol) and the resulting mixture is heated to 90° C. for 1 hour. After cooling, the mixture is suction filtered, the filter residue is thoroughly washed with ether, the filtrate is concentrated in vacuo and the residue is made strongly alkaline with 40% potassium hydroxide solution. It is extracted exhaustively with ether, the extracts obtained are freed from solvent and the remaining residue is distilled in vacuo. The desired compound (93.0 g) is obtained. Boiling point 19 mm Hg 118°-121° C.

WORKUP

后处理

  1. temperatureexternal cooling with ice
  2. temperatureAfter cooling
  3. filtrationfiltered
  4. washthe filter residue is thoroughly washed with ether
  5. concentrationthe filtrate is concentrated in vacuo
  6. extractionIt is extracted exhaustively with ether
  7. customthe extracts obtained
  8. distillationthe remaining residue is distilled in vacuo