反应详情

3.3 Parts of 1-(2,3-dihydro-2,2-dimethyl-4H-1-benzopyran-4-yl)-1H-imidazole-5-carboxylic acid were dissolved in 45 parts of warm N,N-dimethylformamide. After cooling to room temperature, 2 parts of 1,1'-carbonylbis[1H-imidazole] were added and the whole was stirred for 1 hour at this temperature. The whole was heated to ±80° C. and a mixture of 0.1 parts of a cyclohexanol sodium salt solution and 3 parts of cyclohexanol was added. After stirring for 5 days at ±80° C., the mixture was evaporated. The residue was taken up trichloromethane and water and the organic layer was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using trichloromethane as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from hexane. The product was filtered off and dried, yielding 0.91 parts (20.5%) of cyclohexyl 1-(2,3-dihydro-2,2-dimethyl-4H-1-benzopyran-4-yl)-1H-imidazole-5-carboxylate; mp. 128.1° C. (compound 1.139).

1. temperatureThe whole was heated
2. customto ±80° C.
3. additionwas added
4. stirringAfter stirring for 5 days at ±80° C.
5. customthe mixture was evaporated
6. customthe organic layer was dried
7. filtrationfiltered
8. customevaporated
9. customThe residue was purified by column chromatography over silica gel
10. customThe pure fractions were collected
11. customthe eluent was evaporated
12. customThe residue was crystallized from hexane
13. filtrationThe product was filtered off
14. customdried