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
To a mixture of 74 parts of dl-α-(4-methylphenyl)-4-piperidineacetonitrile, 95.4 parts of sodium carbonate, a few crystals of potassium iodide in 1840 parts of 4-methyl-2-pentanone are added portionwise 39.21 parts of (chloromethyl)benzene. After the addition is complete, the whole is stirred and refluxed for 24 hours. The reaction mixture is cooled and 400 parts of water are added. The organic layer is separated, dried over potassium carbonate, filtered and evaporated. The oily residue is dissolved in 1,1'-oxybisethane and gazeous hydrogen chloride is introduced into the solution. The precipitated hydrochloride salt is filtered off and dried, yielding 68 parts of dl-α-(4-methylphenyl)-1-(phenylmethyl)-4-piperidineacetonitrile monohydrochloride; mp. 212°-213° C.
WORKUP
后处理
- additionAfter the addition
- temperaturerefluxed for 24 hours
- temperatureThe reaction mixture is cooled
- customThe organic layer is separated
- dry with materialdried over potassium carbonate
- filtrationfiltered
- customevaporated
- dissolutionThe oily residue is dissolved in 1,1'-oxybisethane
- additiongazeous hydrogen chloride is introduced into the solution
- filtrationThe precipitated hydrochloride salt is filtered off
- customdried