反应详情

温度

110 °C

To a solution of crude 2-(2,3-dihydro-3-methylindol-2-yl)ethylamine (1.75 g) in tetrahydrofuran (12 ml) at room temperature was added in small portions 1,1'-carbonyldiimidazole (1.1 g). After being stirred for 2 hours, the reaction mixture was evaporated in vacuo. The oil obtained was dissolved in toluene (25 ml) and the solution was heated at 110° C. for 1.5 hours. After evaporation of the solvent, the residue was purified by silica gel column chromatography (1% methanol-chloroform) to give crystals. Recrystallization from chloroform-ethyl acetate-hexane gave 3,4,4a,5-tetrahydro-5-methylpyrimido-[1,6-a]indol-1(2H)-one (0.65 g).

1. customthe reaction mixture was evaporated in vacuo
2. customThe oil obtained
3. customAfter evaporation of the solvent
4. customthe residue was purified by silica gel column chromatography (1% methanol-chloroform)
5. customto give crystals
6. customRecrystallization from chloroform-ethyl acetate-hexane