反应详情

To a stirred and heated (90° C.) mixture of 120 parts of piperazine and 400 parts of 1-butanol were added dropwise 60 parts of 3-chloro-7-methyl-1,2-benzisoxazole. Upon complete addition, stirring was continued for 6 hours at reflux temperature. After cooling, the reaction mixture was filtered and the filtrate was evaporated. The residue was taken up in water and the product was extracted with trichloromethane. The extract was dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of trichloromethane and methanol (95:5 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was solidified on standing, yielding 56 parts (71.5%) of 7-methyl-3-(1-piperazinyl)-1,2-benzisoxazole as a residue (int. 2).

1. temperatureheated
2. additionUpon complete addition
3. stirringstirring
4. temperatureat reflux temperature
5. temperatureAfter cooling
6. filtrationthe reaction mixture was filtered
7. customthe filtrate was evaporated
8. extractionthe product was extracted with trichloromethane
9. customThe extract was dried
10. filtrationfiltered
11. customevaporated
12. customThe residue was purified by column chromatography over silica gel using
13. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
14. customThe pure fractions were collected
15. customthe eluent was evaporated