HRID3893

反应详情

EQUATION

反应方程式

HRID 3893 的结构方程式

PROCEDURE

实验过程

4-Amino-1-(naphth-2-ylmethyl)piperidine (1.2 g, 0.005 m) and 2-furoylurea (0.7 g) in pyridine (5 ml) was refluxed for 6 hours, then cooled. Water was added and the precipitate collected by filtration. The solid was dissolved in chloroform with a little methanol and filtered. The solvent was removed under reduced pressure and the residue was purified by medium pressure liquiD chromatography on silica using CHCl3 : MeOH (9:1 v/v) as eluent. The isolated product (1st component eluted) was dissolved in ethyl acetate and acidified with ethanolic HCl to give a precipitate. This was filtered and dried to give 0.3 g of the title compound as the HCl, 3/4H2O salt, mp. 157°-159° C.

WORKUP

后处理

  1. temperaturecooled
  2. filtrationthe precipitate collected by filtration
  3. dissolutionThe solid was dissolved in chloroform with a little methanol
  4. filtrationfiltered
  5. customThe solvent was removed under reduced pressure
  6. customthe residue was purified by medium pressure liquiD chromatography on silica
  7. washThe isolated product (1st component eluted)
  8. dissolutionwas dissolved in ethyl acetate
  9. customto give a precipitate
  10. filtrationThis was filtered
  11. customdried