HRID66671

反应详情

EQUATION

反应方程式

HRID 66671 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. additionAfter the addition
  2. temperaturerefluxed for 24 hours
  3. temperatureThe reaction mixture is cooled
  4. customThe organic layer is separated
  5. dry with materialdried over potassium carbonate
  6. filtrationfiltered
  7. customevaporated
  8. dissolutionThe oily residue is dissolved in 1,1'-oxybisethane
  9. additiongazeous hydrogen chloride is introduced into the solution
  10. filtrationThe precipitated hydrochloride salt is filtered off
  11. customdried