反应详情

To a solution of crude 1-(bromomethyl)-2-chloro-4-nitro-benzene (29.1 mmol; 50% pure) in 30 mL of DCM was added Et3N (4.2 mL, 30 mmol) and 1-methylpiperazine (3.4 mL, 30 mmol). After stirring for 3 h at ambient temperature, aq. NaHCO3 was added and the mixture was extracted with DCM. The combined organic layer was dried over Na2SO4, filtered, concentrated, and the resulting residue was purified by silica gel chromatography (eluted with 5% MeOH/DCM) to provide 6.80 g of product as a dark yellow oil.

1. extractionthe mixture was extracted with DCM
2. dry with materialThe combined organic layer was dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. customthe resulting residue was purified by silica gel chromatography (eluted with 5% MeOH/DCM)