反应详情

温度

120 °C

2-Bromo-6-methyl-4-methoxy-pyridine (202 mg, 1 mmol) was combined with 1,2-ethylenediamine (3 ml) and triethylamin (280 μl, 2 mmol) and heated in a sealed tube at 120° C. for three hours under microwave heating. The mixture was diluted with ethyl acetate, filtered through kieselguhr and evaporated under reduced pressure. The residue was purified by preparative HPLC (Waters XBridge, gradient of water containing 0.1% NH3 and 2% to 100% acetonitrile) to yield 44 mg of a solid (0.24 mmol, 24%) MS(ESI) m/z=182.1 [M+1]+.

1. temperatureheating
2. filtrationfiltered through kieselguhr
3. customevaporated under reduced pressure
4. customThe residue was purified by preparative HPLC (Waters XBridge, gradient of water containing 0.1% NH3 and 2% to 100% acetonitrile)