HRID565394
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
cis-4-(2-methyl-ethyl)-cyclohexyl-amine hydrochloride(60.7 g) was dissolved in ethanol (725 ml). Potassium carbonate (51.8 g) and 1-ethyl-1-methyl-4-oxo-piperidinium iodide (126.6 g) dissolved in water (240 ml) were added and the mixture was refluxed for 1 hour. The reaction mixture was concentrated and extracted three times with dichloromethane. The combined organic layers were washed with aqueous bicarbonate and water, dried (MgSO4) and evaporated. Filtration over silica gel (cyclohexane/ethylacetate 17:3) yielded 69.7 g of a yellow oil which was distilled to yield the title compound (75%) as a slightly yellow oil. b.p. 111° C./0.45 mbar; m/z=223 [M+.].
WORKUP
后处理
- additionwere added
- temperaturethe mixture was refluxed for 1 hour
- concentrationThe reaction mixture was concentrated
- extractionextracted three times with dichloromethane
- washThe combined organic layers were washed with aqueous bicarbonate and water
- dry with materialdried (MgSO4)
- customevaporated
- filtrationFiltration over silica gel (cyclohexane/ethylacetate 17:3)