反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 190 °C
PROCEDURE
实验过程
A mixture of 4 parts of 4,5-dichloro-N1 -{3-[4-(diphenylmethyl)-1-piperazinyl]propyl}-1,2-benzenediamine and 1.5 parts of urea is stirred for 3 hours in an oil-bath at 190° C. After cooling, water and trichloromethane are added. The layers are separated and the organic phase is dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from a mixture of methylbenzene and 2,2'-oxybispropane, yielding 5,6-dichloro-1-{3-[4-(diphenylmethyl)-1-piperazinyl]propyl}-1,3-dihydro-2H-benzimidazol-2-one; mp. 214.7° C.
WORKUP
后处理
- temperatureAfter cooling
- customThe layers are separated
- customthe organic phase is dried
- filtrationfiltered
- customevaporated
- customThe residue is purified by column-chromatography over silica gel using
- additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
- customThe pure fractions are collected
- customthe eluent is evaporated
- customThe residue is crystallized from a mixture of methylbenzene and 2,2'-oxybispropane