HRID46869

反应详情

EQUATION

反应方程式

HRID 46869 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4.6 parts of 1-(3-chloropropyl)-1,3-dihydro-2H-benzimidazol-2-one, 5 parts of 1-(p-fluorophenyl)-1,3,8-triazaspiro[4,5]decan-4-one, 10 parts of sodium carbonate, 0.2 parts of potassium iodide and 80 parts of 4-methyl-2-pentanone is stirred and refluxed overnight. After cooling, the precipitated product is filtered off and triturated twice: first in a boiling mixture of 4-methyl-2-pentanone and 2-propanol and then in boiling methanol. It is filtered off again and crystallized from a mixture of N,N-dimethylformamide and water, yielding 4.5 parts of 8-[3-(1,3-dihydro-2-oxo-2H-benzimidazol-1-yl)propyl]-1-(4-fluorophenyl)-1,3,8-triazaspiro-[4,5]-decan-4-one; mp. 215.4° C.

WORKUP

后处理

  1. temperaturerefluxed overnight
  2. temperatureAfter cooling
  3. filtrationthe precipitated product is filtered off
  4. customtriturated twice
  5. additionfirst in a boiling mixture of 4-methyl-2-pentanone and 2-propanol
  6. filtrationIt is filtered off again
  7. customcrystallized from a mixture of N,N-dimethylformamide and water