反应详情

温度

100 °C

A mixture of N-methylpiperazine (216 mg, 2.15 mmol), 2-bromo-5-nitroanisole (1 g, 4.3 mmol), potassium carbonate (447 mg, 3.23 mmol), copper (I) bromide (86.6 mg, 0.30 mmol) in pyridine (0.5 ml) and toluene (2 ml) was heated at 100° C. overnight. After cooling, the mixture was partitioned between water and ether and the aqueous phase was further extracted with ethyl acetate. The combined organic phases were dried (Na2SO4) and evaporated under reduced pressure, to give the crude product. This was purified by chromatography on silica gel, eluting with methanol and dichloromethane, to give the title compound (D34) as a yellow/brown oil (80 mg, 15%) MH+=252.

1. temperatureAfter cooling
2. customthe mixture was partitioned between water and ether
3. extractionthe aqueous phase was further extracted with ethyl acetate
4. dry with materialThe combined organic phases were dried (Na2SO4)
5. customevaporated under reduced pressure
6. customto give the crude product
7. customThis was purified by chromatography on silica gel
8. washeluting with methanol and dichloromethane