反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
4-Amino-1-(4-phenyl-4-oxobutyl)piperidine dihydrochloride (3.19 g.) was stirred in chloroform (50 ml.). Water (20 ml.) containing potassium carbonate (8.28 g.) was added followed by dropwise addition of piperonyl chloride (1.84 g.) in chloroform (10 ml.). The mixture was stirred for 18 hr. Some of the title compound separated as the free base and was filteredoff. The two-phase filtrate was separated and the remainder of the title compound (base) obtained. The combined bases were dissolved in ethanol/HCland ether added until crystallisation occurred. Filtration afforded the title compound as the hydrochloride, three-quarter hydrate, colourless prisms (3.876 g.), m.p. 235.7°. Analysis: Found: C, 62.19; H, 6.28;N, 6.33. C23H26N2O4.HCl.3/4H2O. C, 62.15; H, 6.47; N, 6.13%.
WORKUP
后处理
- additionwas added
- customSome of the title compound separated as the free base
- customThe two-phase filtrate was separated