HRID464956

反应详情

EQUATION

反应方程式

HRID 464956 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 108.68 g (2.860 mole) lithium aluminum hydride in 800 ml tetrahydrofuran, is added a solution of 194.5 g (0.790 mole) of N-ethyl-5-oxo-1-(phenylmethyl)-3-pyrrolidinecarboxamide in 600 ml tetrahydrofuran dropwise under nitrogen. The reaction was then refluxed four hours. The reaction flask was cooled in an ice bath and 108 ml of water, 108 ml of 15% sodium hydroxide, and 324 ml of water were added. The precipitated solids were filtered and washed with hot ethanol. The combined filtrates were concentrated, then dissolved in dichloromethane, filtered, dried over magnesium sulfate, and the solvent evaporated under reduced pressure to give 151.9 g of N-ethyl-1-(phenylmethyl)-3-pyrrolidinemethanamine as an oil.

WORKUP

后处理

  1. temperatureThe reaction was then refluxed four hours
  2. temperatureThe reaction flask was cooled in an ice bath
  3. filtrationThe precipitated solids were filtered
  4. washwashed with hot ethanol
  5. concentrationThe combined filtrates were concentrated
  6. dissolutiondissolved in dichloromethane
  7. filtrationfiltered
  8. dry with materialdried over magnesium sulfate
  9. customthe solvent evaporated under reduced pressure