反应详情

温度

70 °C

A mixture of 11.3 parts of 6-(2-chloroethyl)-1,7-dimethylimidazo[1,2-a]pyrimidin-5(1H)-one (interm. 15), 18.9 parts of N-(4-piperidinyl)-1H-benzimidazol-2-amine dihydrobromide, 16 parts of sodium carbonate, 0.01 parts of potassium iodide and 376 parts of N,N-dimethylacetamide was stirred overnight at 70° C. The reaction mixture was filtered and the filtrate was evaporated. The residue was taken up in a mixture of water, dichloromethane and methanol. The organic layer was separated and the aqueous layer was re-extracted with a mixture of dichloromethane and methanol. The combined organic layers were dried, filtered and evaporated. The residue was crystallized from ethanol, yielding 17.5 parts (86.3%) of 6-[2-[4-(1H-benzimidazol-2-ylamino)-1-piperidinyl]-ethyl]-1,7-dimethylimidazo[1,2-a]pyrimidin-5(1H)-one; mp. 229.5° C. (comp. 80).

1. filtrationThe reaction mixture was filtered
2. customthe filtrate was evaporated
3. additionThe residue was taken up in a mixture of water, dichloromethane and methanol
4. customThe organic layer was separated
5. extractionthe aqueous layer was re-extracted with a mixture of dichloromethane and methanol
6. customThe combined organic layers were dried
7. filtrationfiltered
8. customevaporated
9. customThe residue was crystallized from ethanol