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
A mixture of 2.46 g. of 1-(p-chlorophenylsulfinyl)-3-chloropropane, 0.9 g. of piperidine, 0.53 g. of sodium carbonate in 30 ml. of dimethylformamide is heated for 3 hours at a temperature of 80° - 87°C. After the reaction mixture has been cooled, a mixture of benzene and water is added thereto. The aqueous layer is separated and extracted with benzene. The organic layers are combined, washed with water, dried over sodium sulfate and evaporated under reduced pressure. The oily residue is dissolved in ether and treated with ethanolic hydrogen chloride under cooling. The precipitate is collected by filtration and dried to give 1-[γ-(p-chlorophenylsulfinyl)-propyl]piperidine hydrochloride, m.p.: 170° - 174°C. Recrystallization from benzene gives white crystals, m.p.: 176° - 177°C.
WORKUP
后处理
- additionA mixture of 2.46 g
- temperatureAfter the reaction mixture has been cooled
- additionis added
- customThe aqueous layer is separated
- extractionextracted with benzene
- washwashed with water
- dry with materialdried over sodium sulfate
- customevaporated under reduced pressure
- dissolutionThe oily residue is dissolved in ether
- additiontreated with ethanolic hydrogen chloride
- temperatureunder cooling
- filtrationThe precipitate is collected by filtration
- customdried