反应详情

To 60 mL of toluene was added 4.0 g (0.0152 mol) of 4-(2-chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one, 6.0 g (0.033 mol) of 1-(2-pyrimidyl)piperazine, and 4.0 g (0.04 mol) of triethylamine. The reaction mixture was heated at reflux for 2 days and subsequently washed with 2×50 mL of 1N NaOH, dried over Na2SO4, filtered, and concentrated by rotary evaporation. Crystallization from ethyl acetate afforded 4.0 g, 67% of analytically pure crystals, mp 161°-62° C.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 2 days
3. washsubsequently washed with 2×50 mL of 1N NaOH
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated by rotary evaporation
7. customCrystallization from ethyl acetate
8. customafforded 4.0 g, 67% of analytically pure crystals, mp 161°-62° C.