反应详情

温度

80 °C

A mixture of 3.4 parts of 7-[chlorophenylmethyl]quinoline, 4.5 parts of 1H-imidazole and 72 parts of N,N-dimethylformamide was stirred for 6 hours at 80° C. The reaction mixture was evaporated to dry and the residue was taken up in water. The product was extracted three times with 65 parts of dichloromethane. The combined extracts were dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of dichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from a mixture of 2,2'-oxybispropane and 2-propanone. The product was filtered off and dried, yielding 1.27 parts (33.2%) of 7-[(1H-imidazol-1yl)phenylmethyl]quinoline; mp. 110.7° C.(compound 26).

1. customThe reaction mixture was evaporated
2. customto dry
3. extractionThe product was extracted three times with 65 parts of dichloromethane
4. customThe combined extracts were dried
5. filtrationfiltered
6. customevaporated
7. customThe residue was purified by column chromatography over silica gel using
8. additiona mixture of dichloromethane and methanol (95:5 by volume) as eluent
9. customThe pure fractions were collected
10. customthe eluent was evaporated
11. customThe residue was crystallized from a mixture of 2,2'-oxybispropane and 2-propanone
12. filtrationThe product was filtered off
13. customdried