反应详情

A mixture of 2.28 parts of 2,6-dichloro-α-(4-chlorophenyl)-4-(4,5-dihydro-3,5-dioxo-1,2,4-triazin-2(3H)-yl)benzeneacetylchloride, 4.5 parts of pyrrolidine and 40 parts of acetonitrile was stirred for 17 hours at room temperature. After evaporation in vacuo, the residue was taken up in water and the mixture was acidified with hydrochloric acid. 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 dried in vacuo for 48 hours at 110° C., yielding 0.8 parts (36.2%) of 1-[2-(4-chlorophenyl)-2-[2,6-dichloro-4-(4,5-dihydro-3,5-dioxo-1,2,4-triazin-2(3H)-yl)phenyl]acetyl]pyrrolidine; mp. 153.9° C. (intermediate 35).

1. customAfter evaporation in vacuo
2. extractionThe product was extracted with trichloromethane
3. customThe extract was dried
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified by column chromatography over silica gel using
7. additiona mixture of trichloromethane and methanol (95:5 by volume) as eluent
8. customThe pure fractions were collected
9. customthe eluent was evaporated
10. customThe residue was dried in vacuo for 48 hours at 110° C.