HRID66673

反应详情

EQUATION

反应方程式

HRID 66673 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To 5 parts of magnesium are added 2.18 parts of 1,2-dibromoethane and a small amount of iodine to initiate the reaction. Then there is added dropwise a solution of 28 parts of 4-chloro-1-methylpiperidine in 180 parts of tetrahydrofuran while the mixture is heated to 70° C. After cooling, there is added dropwise a solution of 14 parts of 3-methylbenzonitrile in 90 parts of tetrahydrofuran. Upon completion, stirring is continued for 1 hour at reflux temperature. The reaction mixture is cooled and poured onto a solution of 75 parts of ammonium chloride in water. The product is extracted with 2,2'-oxybispropane. The extract is washed with water, dried, filtered and evaporated, yielding 35 parts of (3-methylphenyl) (1-methyl-4-piperidinyl)methanone as an oily residue.

WORKUP

后处理

  1. customthe reaction
  2. temperatureAfter cooling
  3. temperatureat reflux temperature
  4. temperatureThe reaction mixture is cooled
  5. extractionThe product is extracted with 2,2'-oxybispropane
  6. washThe extract is washed with water
  7. customdried
  8. filtrationfiltered
  9. customevaporated