反应详情

To a stirred mixture of 3 parts of 2,6-dichloro-α-(4-chlorophenyl)-4-(3,4,5,6-tetrahydro-4-methyl-3,5-dioxo-1,2,4-triazin-2(1H)-yl)benzeneacetonitrile and 20 parts of pyridine were added dropwise 1.7 parts of benzoyl chloride during a period of 5 minutes at room temperature and under nitrogen atmosphere. Upon complete addition, stirring was continued overnight at room temperature. The reaction mixture was evaporated in vacuo and the residue was stirred in water. The product was extracted with trichloromethane. The extract was dried, filtered and evaporated. The residue was purified twice by column chromatography over silica gel using trichloromethane as eluent. The pure fractions were collected and the eluent was evaporated in vacuo. The residue was crystallized from 8 parts of acetonitrile. The product was filtered off, washed with 2,2'-oxybispropane and dried, yielding 0.8 parts (20.2%) of 1-benzoyl-2-[3,5-dichloro-4-[(4-chlorophenyl)cyanomethyl]phenyl]-1,6-dihydro-4-methyl-1,2,4-triazine-3,5(2H,4H)-dione; mp. 148.4° C. (compound 79).

1. additionUpon complete addition
2. customThe reaction mixture was evaporated in vacuo
3. stirringthe residue was stirred in water
4. extractionThe product was extracted with trichloromethane
5. customThe extract was dried
6. filtrationfiltered
7. customevaporated
8. customThe residue was purified twice by column chromatography over silica gel
9. customThe pure fractions were collected
10. customthe eluent was evaporated in vacuo
11. customThe residue was crystallized from 8 parts of acetonitrile
12. filtrationThe product was filtered off
13. washwashed with 2,2'-oxybispropane
14. customdried