HRID256179

反应详情

EQUATION

反应方程式

HRID 256179 的结构方程式

PROCEDURE

实验过程

A mixture of 2-(5-chloro-2-nitrophenyl)-1,3-dioxolane (21.3 g, 0.09 mole) and piperidine (39.6 g, 0.46 mole) was heated at reflux in an oil bath. After 3 hours, excess piperidine was evaporated and the residue partitioned between water and dichloromethane. The organic phase was separated and the aqueous layer extracted with dichloromethane. Combined extracts were washed with water, dried over magnesium sulfate and concentrated in vacuo to afford 2-(2-nitro-5-piperdinylphenyl)-1,3-dioxolane (21.6 g, 100%) as a dark colored oil which was used without further purification. An analytical sample was purified by flash chromatography using dichloromethane as eluant to give a light yellow oil.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux in an oil bath
  3. customexcess piperidine was evaporated
  4. customthe residue partitioned between water and dichloromethane
  5. customThe organic phase was separated
  6. extractionthe aqueous layer extracted with dichloromethane
  7. washCombined extracts were washed with water
  8. dry with materialdried over magnesium sulfate
  9. concentrationconcentrated in vacuo