反应详情

温度

60 °C

To 20 mL of morpholine 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 in 60° C. for 24 hrs. The excess morpholine was removed by rotary evaporation and finally by high vacuum (0.5 mm Hg ~60° C.). The residue was dissolved in ~100 mL of CH2Cl2 washed with 3×50 ml of 1N NaOH, dried over Na2SO4, filtered, and concentrated by rotary evaporation. The residue was crystallized from isopropyl ether to give 2.7 g (65%) of analytically pure crystals, mp 111°-12° C.

1. customThe excess morpholine was removed by rotary evaporation and finally by high vacuum (0.5 mm Hg ~60° C.)
2. dissolutionThe residue was dissolved in ~100 mL of CH2Cl2
3. washwashed with 3×50 ml of 1N NaOH
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated by rotary evaporation
7. customThe residue was crystallized from isopropyl ether
8. customto give 2.7 g (65%) of analytically pure crystals, mp 111°-12° C.