反应详情

To a stirred and refluxed solution of 1.5 parts of 2,6-dichloro-α-(4-chlorophenyl)-4-(4,5-dihydro-3,5-dioxo-1,2,4-triazin2(3H)-yl)benzeneacetic acid in 100 parts of acetic acid were added 3 parts of zinc. Stirring was continued for 30 minutes at reflux temperature. The zinc salts were filtered off and the filtrate was evaporated. The residue was washed with water whereupon the solid product was filtered off and dissolved in a mixture of trichlorometmhane and methanol (90:10 by volume). The solution was dried, filtered and evaporated. The residue was washed with ethyl acetate and 2,2'-oxybispropane and dried, yielding 0.98 parts (67.2%) of 2,6-dichloro-α-(4-chlorophenyl)-4-(3,4,5,6-tetrahydro-3,5-dioxo-1,2,4-triazin-2(1H)-yl)benzeneacetic acid; mp. 194.2° C. (compound 1).

1. stirringStirring
2. temperatureat reflux temperature
3. filtrationThe zinc salts were filtered off
4. customthe filtrate was evaporated
5. washThe residue was washed with water whereupon the solid product
6. filtrationwas filtered off
7. dissolutiondissolved in a mixture of trichlorometmhane and methanol (90:10 by volume)
8. customThe solution was dried
9. filtrationfiltered
10. customevaporated
11. washThe residue was washed with ethyl acetate and 2,2'-oxybispropane
12. customdried