HRID1165569

反应详情

EQUATION

反应方程式

HRID 1165569 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1,000 g (5.34 mols) of 1-benzyl-Δ3 -pyrroline-2,5-dione are dissolved in 2.5 l of tetrahydrofuran, and 572 g (5.34 mols) of benzylamine are added with stirring at 10° to 20° C. The mixture is left to stand for 24 hours at room temperature, after which 360 g are removed from the resulting solution (3,848 g of total weight) and added to a solution of 38 g (1 mol) of lithium aluminum hydride in 380 ml of absolute dehydrated tetrahydrofuran. The mixture is refluxed for 20 hours, 500 ml of tetrahydrofuran, 38 g of water and 120 ml of tetrahydrofuran, 38 g of 10% strength potassium hydroxide solution and 114 g of water are then sucessively added to the mixture. The salts are filtered off with suction, washed with tetrahydrofuran, the filtrate is concentrated, and the residue is distilled.

WORKUP

后处理

  1. waitThe mixture is left
  2. customafter which 360 g are removed from the resulting solution (3,848 g of total weight)
  3. temperatureThe mixture is refluxed for 20 hours
  4. filtrationThe salts are filtered off with suction
  5. washwashed with tetrahydrofuran
  6. concentrationthe filtrate is concentrated
  7. distillationthe residue is distilled