HRID2296384

反应详情

EQUATION

反应方程式

HRID 2296384 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

60 g of hydrazodicarbonamide and 56 g of n-hexylamine are stirred in 100 ml of N-methy pyrrolidone for 6 hours at 150° C., for 20 hours at 175° C. and for 20 hours at 180° C. The solvent is then distilled off in vacuo and the residue is triturated with 100 ml of 10% sodium hydroxide solution. The deposit is isolated by filtration under suction and the filtrate is neutralised with 10% hydrochloric acid. A deposit is precipitated and is isolated by filtration under suction, washed with water and dried in vacuo, giving 75 g (81% of the theoretical yield) of 4-(n-hexyl)-1,2,4-triazolidine-3,5-dione in the form of colourless crystals melting at 144° C. to 145° C.

WORKUP

后处理

  1. distillationThe solvent is then distilled off in vacuo
  2. customthe residue is triturated with 100 ml of 10% sodium hydroxide solution
  3. customThe deposit is isolated by filtration under suction
  4. customA deposit is precipitated
  5. customis isolated by filtration under suction
  6. washwashed with water
  7. customdried in vacuo
  8. customgiving 75 g (81% of the