反应详情

To a solution of 2-chloro-5-[4-(2-dimethylaminoethyl)-piperazin-1-yl]-benzoic acid (0.40 g, 1.29 mmol) in dry DMF (5 mL) was added 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) (0.25 g, 1.29 mmol), followed by 1-hydroxybenzotriazole hydrate (1-HOBt) (0.11 g, 0.77 mmol) and dimethyl-pyridin-4-yl-amine (DMAP) (0.08 g, 0.64 mmol). After 3 h stirring at room temperature, 1,2-phenylenediamine (0.21 g, 1.93 mmol) was added, and the resulting mixture was stirred at room temperature overnight. The solution was evaporated under reduced pressure, then diluted with dichlomethane (20 mL) and washed with saturated Na2CO3 solution (2×5 mL). The organic layer was dried over Na2SO4, filtered and evaporated under reduced pressure. The resulting solid was purified by flash chromatography (eluent:dichloromethane:MeOH:NH3 in MeOH (2M)/9:0.5:0.5) to obtain 0.18 g (35%) of the title compound.

1. stirringthe resulting mixture was stirred at room temperature overnight
2. customThe solution was evaporated under reduced pressure
3. additiondiluted with dichlomethane (20 mL)
4. washwashed with saturated Na2CO3 solution (2×5 mL)
5. dry with materialThe organic layer was dried over Na2SO4
6. filtrationfiltered
7. customevaporated under reduced pressure
8. customThe resulting solid was purified by flash chromatography (eluent:dichloromethane:MeOH:NH3 in MeOH (2M)/9:0.5:0.5)