反应详情

温度

60 °C

To 20 mL of N-methylpiperazine was added 3.0 g (0.01 mol) of 2-(2-chloroethyl)-3,4-dihydro-1,4-dimethyl-1H-[1,3,5]triazepino[3,2-a]benzimidazol-5(2H)-one. The reaction mixture was heated to 60° C. for 24 hr. The excess amine was removed at 70° C., 0.5 mm Hg. The residual oil was taken up in 60 mL of CH2Cl2 and washed with 2×50 mL of 1N NaOH. The organic layer was dried over Na2SO4, filtered, concentrated by rotary evaporation, and further concentrated at 90° C., 0.5 mm Hg. The residual oil/glass was treated with 2 equivalent of fumaric acid isopropyl alcohol to give 3.4 g of solid. This was recrystallized from isopropyl alcohol to give 3.0 g (51%) off-white analytically pure material, mp 171°-79° C.

1. customThe excess amine was removed at 70° C.
2. washwashed with 2×50 mL of 1N NaOH
3. dry with materialThe organic layer was dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated by rotary evaporation
6. concentrationfurther concentrated at 90° C.