反应详情

To a stirred mixture of 6-(4-aminophenyl)-5-methyl-4,5-dihydro-1,2,4-triazin-3(2H)-one (1.0 g) and N,N-dimethylaniline (0.93 ml) in DMF (10 ml) was added dropwise 2-acetoxypropionyl chloride (0.98 g) under ice cooling. The stirring was continued for one night at ambient temperature. The mixture was concentrated under reduced pressure. The residue was extracted with ethyl acetate after addition of saline solution. The extract was washed successively with 1N hydrochloric acid, water and saline solution, dried over magnesium sulfate and evaporated in vacuo. The residue was chromatographed on silica gel (170 ml) with a mixture of chloroform and methanol (10:1) as an eluent. The eluates containing the object compound were evaporated in vacuo to give 1.13 g of 6-[4-(2-acetoxypropionylamino)phenyl]-5-methyl-4,5-dihydro-1,2,4-triazin-3(2H)-one.

1. waitThe stirring was continued for one night at ambient temperature
2. concentrationThe mixture was concentrated under reduced pressure
3. extractionThe residue was extracted with ethyl acetate
4. additionafter addition of saline solution
5. washThe extract was washed successively with 1N hydrochloric acid, water and saline solution
6. dry with materialdried over magnesium sulfate
7. customevaporated in vacuo
8. customThe residue was chromatographed on silica gel (170 ml) with a mixture of chloroform and methanol (10:1) as an eluent
9. additionThe eluates containing the object compound
10. customwere evaporated in vacuo