HRID256179
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperaturewas heated
- temperatureat reflux in an oil bath
- customexcess piperidine was evaporated
- customthe residue partitioned between water and dichloromethane
- customThe organic phase was separated
- extractionthe aqueous layer extracted with dichloromethane
- washCombined extracts were washed with water
- dry with materialdried over magnesium sulfate
- concentrationconcentrated in vacuo