反应详情

温度

70 °C

A mixture of 0.9 parts of morpholine, 4.8 parts of N-[1-(2-chloroethyl)-4-piperidinyl]-1-(4-fluorophenylmethyl)-1H-benzimidazol-2-amine dihydrochloride, 3 parts of sodium carbonate, 0.1 parts of potassium iodide and 135 parts of N,N-dimethylformamide is stirred and heated overnight at 70° C. The reaction mixture is poured onto water and the product is extracted with methylbenzene. The extract is dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (98:2 by volume) as eluent. The pure fractions are collected and the eluent is evaporated. The residue is crystallized from a mixture of 2-propanone and 2,2'-oxybispropane, yielding 0.6 parts (12.5%) of [2-{4-[1-(4-fluorophenylmethyl)-1H-benzimidazol-2-ylamino]-1-piperidinyl}ethyl] 4-morpholinecarboxylate; mp. 144.8° C.

1. additionThe reaction mixture is poured onto water
2. extractionthe product is extracted with methylbenzene
3. customThe extract is dried
4. filtrationfiltered
5. customevaporated
6. customThe residue is purified by column-chromatography over silica gel using
7. additiona mixture of trichloromethane and methanol (98:2 by volume) as eluent
8. customThe pure fractions are collected
9. customthe eluent is evaporated
10. customThe residue is crystallized from a mixture of 2-propanone and 2,2'-oxybispropane