HRID236739

反应详情

EQUATION

反应方程式

HRID 236739 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a warm solution of 192 parts of ethyl 4-[(4-chlorophenyl)imino]-1-piperidinecarboxylate in 560 parts of methanol is added portionwise 23.5 parts of sodium borohydride at 50° C. and over a period of one hour. After the addition is complete, the mixture is stirred at the same temperature for 2 hours. The methanol is evaporated. The solid residue is heated with ±600 parts of water and the product is extracted with benzene. The extract is dried over magnesium sulfate and evaporated. The oily residue solidifies on treating with 2,2'-oxybispropane. The solid is filtered off and dried, yielding 122 parts of ethyl 4-[(4-chlorophenyl)amino]-1-piperidinecarboxylate; mp. 115°-118° C.

WORKUP

后处理

  1. additionAfter the addition
  2. customThe methanol is evaporated
  3. temperatureThe solid residue is heated with ±600 parts of water
  4. extractionthe product is extracted with benzene
  5. dry with materialThe extract is dried over magnesium sulfate
  6. customevaporated
  7. additionon treating with 2,2'-oxybispropane
  8. filtrationThe solid is filtered off
  9. customdried