HRID565394

反应详情

EQUATION

反应方程式

HRID 565394 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. additionwere added
  2. temperaturethe mixture was refluxed for 1 hour
  3. concentrationThe reaction mixture was concentrated
  4. extractionextracted three times with dichloromethane
  5. washThe combined organic layers were washed with aqueous bicarbonate and water
  6. dry with materialdried (MgSO4)
  7. customevaporated
  8. filtrationFiltration over silica gel (cyclohexane/ethylacetate 17:3)