HRID1587293

反应详情

EQUATION

反应方程式

HRID 1587293 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

54 g (0.16 mol) of 4-phthalimidomethyl-1-benzyl-pyrrolidin-2-one are stirred into 1.3 l of ethyl alcohol after the addition of 32 g of hydrazine hydrate for 4 hours at room temperature. The precipitate (phthalic acid hydrazide) is removed by suction filtering the filtrate is evaporated down. 500 ml of methylene choloride are added to the residue which is then extracted three times with 100 ml of water. The organic phase is dried and evaporated down. The residue remaining is dissolved in 500 ml of methanol and 20 g (0.17 mol) of solid fumaric acid are added in batches thereto, with stirring, at boiling temperature. As the mixture cools, colorless crystals are precipitated, which are then suction filtered and washed with methanol and ether.

WORKUP

后处理

  1. customThe precipitate (phthalic acid hydrazide) is removed by suction
  2. filtrationfiltering the filtrate
  3. customis evaporated down
  4. addition500 ml of methylene choloride are added to the residue which
  5. extractionis then extracted three times with 100 ml of water
  6. customThe organic phase is dried
  7. customevaporated down
  8. dissolutionThe residue remaining is dissolved in 500 ml of methanol
  9. customcolorless crystals are precipitated
  10. filtrationsuction filtered
  11. washwashed with methanol and ether