HRID1418840

反应详情

EQUATION

反应方程式

HRID 1418840 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A sample of the product of step (a), 17 g, was dissolved in 200 ml of 1M hydrochloric acid. The mixture was then hydrogenated with 1 g of 5% Pd/C. When hydrogen uptake had stopped the catalyst was filtered off. The solvent was evaporated in vacuum, and the residue dissolved in isopropanol, evaporated in vacuum again and the residue dissolved in 100 ml of methanol. To this mix was added 200 ml of toluene. This was then concentrated on a steam bath until the volume had decreased to approximately 175 ml. The crystals that precipitated were filtered to give N-(3-aminophenyl)-1-pyrrolidinecarboximidamide dihydrochloride, m.p. 250°-251° C.

WORKUP

后处理

  1. filtrationwas filtered off
  2. customThe solvent was evaporated in vacuum
  3. dissolutionthe residue dissolved in isopropanol
  4. customevaporated in vacuum again
  5. dissolutionthe residue dissolved in 100 ml of methanol
  6. additionTo this mix was added 200 ml of toluene
  7. concentrationThis was then concentrated on a steam bath until the volume
  8. customThe crystals that precipitated
  9. filtrationwere filtered