HRID1164356

反应详情

EQUATION

反应方程式

HRID 1164356 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a stirred and hot solution of 8.5 parts of N,N,N-triethylbenzenemethanaminium chloride, 40 parts of sodium hydroxide and 360 parts of a sodium hydroxide solution 50%, is added dropwise a solution of 72.7 parts of N,N-bis(2-chloroethyl)-4-methylbenzenesulfonamide and 45.5 parts of 2,4-dichlorobenzeneacetonitrile in 90 parts of tetrahydrofuran. Upon completion, stirring is continued for 3 hours at 50° C. The reacton mixture is cooled, 216 parts of methylbenzene and 480 parts of water are added and the layers are separated. The organic phase is washed with water, dried, filtered and evaporated. The residue is crystallized from 2-propanol, yielding 28 parts (29%) of 4-(2,4-dichlorophenyl)-1-(4-methylphenylsulfonyl)-4-piperidinecarbonitrile; mp. 145° C.

WORKUP

后处理

  1. stirringUpon completion, stirring
  2. temperatureThe reacton mixture is cooled
  3. customthe layers are separated
  4. washThe organic phase is washed with water
  5. customdried
  6. filtrationfiltered
  7. customevaporated
  8. customThe residue is crystallized from 2-propanol