反应详情

Cyclopropanecarbonyl chloride (0.47 g) was added dropwise to a stirred solution of 6-(1,2,3,4-tetrahydroquinolin-6-yl)-5-methyl-4,5-dihydro-1,2,4-triazin-3(2H)-one (0.73 g) and triethylamine (0.6 g) in N,N-dimethylformamide (7.3 ml) under ice cooling and the stirring was continued for 30 minutes. The solution was evaporated in vacuo and the residue was dissolved in chloroform. The solution was washed with diluted hydrochloric acid, dried, and evaporated. The residue was chromatographed on silica gel (5 g) using chloroform and then a mixture of chloroform and methanol (20:1) as an eluents. The eluates were evaporated in vacuo and the oily residue was crystallized from ethanol to give 6-(1-cyclopropanecarbonyl-1,2,3,4-tetrahydroquinolin-6-yl)-5-methyl-4,5-dihydro-1,2,4-triazin-3(2H)-one (0.26 g).

1. customThe solution was evaporated in vacuo
2. dissolutionthe residue was dissolved in chloroform
3. washThe solution was washed with diluted hydrochloric acid
4. customdried
5. customevaporated
6. customThe residue was chromatographed on silica gel (5 g)
7. additiona mixture of chloroform and methanol (20:1) as an eluents
8. customThe eluates were evaporated in vacuo
9. customthe oily residue was crystallized from ethanol