反应详情

To 90 mL of freshly collected dimethylamine and 10 mL of methanol was added 3.25 g (0.011 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 flask was sealed and left standing at room temperature for 6 days. The dimethylamine was then allowed to evaporate at room temperature and the residue partitioned between 75 mL of 1N NaOH and 75 mL of CH2Cl2. The organic phase was washed with another 50 mL of 1N NaOH. The combined organic layers were dried over Na2SO4, filtered, and concentrated by rotary evaporation. The solid residue was recrystallized from isopropyl ether to give 2.8 g of white analytically pure crystals, mp 91°-95° C.

1. customThe reaction flask was sealed
2. waitleft
3. customto evaporate at room temperature
4. customthe residue partitioned between 75 mL of 1N NaOH and 75 mL of CH2Cl2
5. washThe organic phase was washed with another 50 mL of 1N NaOH
6. dry with materialThe combined organic layers were dried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated by rotary evaporation
9. customThe solid residue was recrystallized from isopropyl ether
10. customto give 2.8 g of white analytically pure crystals, mp 91°-95° C.