反应详情

A solution of 1 g (3.78 mmol) 1-bromomethyl-2-methyl-4-nitro-benzene, 0.539 ml (4.16 mmol) 1-ethylpiperazine and 0.63 ml (4.54 mmol) triethylamine in 15 ml dichloromethane is stirred at room temperature for 0.5 h. Then the reaction mixture is poured on water and extracted 3× with EtOAc. The combined organic layers are washed with water and saturated NaCl solution, dried over MgSO4, filtered and the filtrate is concentrated in vacuo. The residue is purified by chromatography (silicagel, 100% EtOAc=>EtOAc:MeOH=7:3) to afford the title compound as a solid.

1. additionThen the reaction mixture is poured on water
2. extractionextracted 3× with EtOAc
3. washThe combined organic layers are washed with water and saturated NaCl solution
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationthe filtrate is concentrated in vacuo
7. customThe residue is purified by chromatography (silicagel, 100% EtOAc=>EtOAc:MeOH=7:3)