HRID3893
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperaturecooled
- filtrationthe precipitate collected by filtration
- dissolutionThe solid was dissolved in chloroform with a little methanol
- filtrationfiltered
- customThe solvent was removed under reduced pressure
- customthe residue was purified by medium pressure liquiD chromatography on silica
- washThe isolated product (1st component eluted)
- dissolutionwas dissolved in ethyl acetate
- customto give a precipitate
- filtrationThis was filtered
- customdried