反应详情

温度

90 °C

To 15 mL of N-methylaniline was added 3.5 g (0.0133 mol) of 4-(2-chloroethyl)-3,4-dihydro-2-methylpyrimido[1,6-a]benzimidazol-1(2H)-one. The reaction mixture was heated to 90° C. (oil bath) for 2 days, and the excess N-methylaniline removed in vacuo at 80° C., 0.5 mm Hg. The residue was dissolved in 100 mL of CH2Cl2, washed with 2×100 mL of 1N NaOH, dried over Na2SO4, filtered, and concentrated by rotary evaporation. The residue was subjected to high vacuum (0.5 mm, Hg) at 85° C. for 2 hr, and then crystallized from iso-octane/toluene to give 2.3 g (52%) of analytically pure crystals, mp 130°-31° C.

1. customthe excess N-methylaniline removed in vacuo at 80° C.
2. dissolutionThe residue was dissolved in 100 mL of CH2Cl2
3. washwashed with 2×100 mL of 1N NaOH
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated by rotary evaporation
7. customcrystallized from iso-octane/toluene
8. customto give 2.3 g (52%) of analytically pure crystals, mp 130°-31° C.