HRID1154729

反应详情

EQUATION

反应方程式

HRID 1154729 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 cooled (ice-bath) mixture of 5 parts of N,N'-methanetetraylbis[cyclohexanamine], 25.2 parts of carbon disulfide and 40 parts of pyridine are added 6 parts of 4-[4-(4-methoxyphenyl)-1-piperazinyl]benzenamine and the whole is stirred first for 1 hour in an ice-bath and further for 2 hours at room temperature. 35 Parts of 2,2'-oxybispropane are added and the whole is stirred for 30 minutes. The precipitated product is filtered off and crystallized from 4-methyl-2-pentanone. The product is filtered off again and recrystallized from 1,4-dioxane, yielding 2.45 parts of 1-(4-isothiocyanatophenyl)-4-(4-methoxyphenyl)piperazine; mp. 180.6° C.

WORKUP

后处理

  1. temperaturecooled
  2. stirringthe whole is stirred first for 1 hour in an ice-bath and further for 2 hours at room temperature
  3. stirringthe whole is stirred for 30 minutes
  4. filtrationThe precipitated product is filtered off
  5. customcrystallized from 4-methyl-2-pentanone
  6. filtrationThe product is filtered off again
  7. customrecrystallized from 1,4-dioxane