反应详情

A mixture of 1-chloro-4-methoxy-5-nitro-2-vinylbenzene (0.42 g, 1.95 mmol), 4-(4-methyl-piperazin-1-yl)-benzylamine (1.2 g, 5.85 mmol) and quinol (0.043 g, 0.39 mmol) in n-butanol (8 mL) was heated to reflux for 12 hours under a N2 atmosphere. Water (100 mL) was added and the reaction mixture extracted with EtOAc (3×100 mL). The combined organic extracts were washed with brine (50 mL), dried (Na2SO4) and concentrated under reduced pressure. The residue was purified by column chromatography on neutral silica gel using 3-5% methanol in DCM to give the title compound (0.35 g, 43%) as a solid.

1. temperaturewas heated
2. temperatureto reflux for 12 hours under a N2 atmosphere
3. extractionthe reaction mixture extracted with EtOAc (3×100 mL)
4. washThe combined organic extracts were washed with brine (50 mL)
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated under reduced pressure
7. customThe residue was purified by column chromatography on neutral silica gel using 3-5% methanol in DCM