反应详情

温度

130 °C

The mixture of 2-((6-methyl-3-(methylthio)-5-oxo-1,2,4-triazin-4(5H)-yl)methyl)benzonitrile (6, 68 mg, 0.25 mmol) and (R)-tert-butyl piperidin-3-ylcarbamate (60 mg, 0.30 mmol) was ground for 5 min and then heated in a tube under nitrogen atmosphere at 130° C. for 13 h. The mixture was separated by silica gel column, and eluted with 2:1 to 1:1 petroleum ether-ethyl acetate and then with 1:1:2 petroleum ether-dichloromethane-ethyl acetate to give (R)-tert-butyl 1-(4-(2-cyanobenzyl)-6-methyl-5-oxo-4,5-dihydro-1,2,4-triazin-3-yl)piperidin-3-ylcarbamate (7). MS: m/z, 425 (100%, M+1), 447(40%, M+23).

1. customThe mixture was separated by silica gel column
2. washeluted with 2:1 to 1:1 petroleum ether-ethyl acetate