HRID28128

反应详情

EQUATION

反应方程式

HRID 28128 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred and refluxing mixture of 250 parts of ethyl 4-[(2,6-dichlorophenyl)imino]-1-piperidinecarboxylate in 160 parts of methanol and 160 parts of 2-propanol are added portionwise 30 parts of sodium borohydride. Upon completion, stirring at reflux temperature is continued for one hour. The warm reaction mixture is poured onto water and the product is extracted with methylbenzene. The extract is dried and evaporated. The residue is crystallized from a mixture of 160 parts of 2,2'-oxybispropane and 160 parts of petroleumether, yielding 96 parts of ethyl 4-[(2,6-dichlorophenyl)-amino]-1-piperidinecarboxylate; mp. 107.2°-116.6° C.

WORKUP

后处理

  1. temperaturerefluxing
  2. stirringUpon completion, stirring
  3. temperatureat reflux temperature
  4. customThe warm reaction mixture
  5. additionis poured onto water
  6. extractionthe product is extracted with methylbenzene
  7. customThe extract is dried
  8. customevaporated
  9. customThe residue is crystallized from a mixture of 160 parts of 2,2'-oxybispropane and 160 parts of petroleumether