反应详情

2,4-Dichloro-5-phenyl-thieno[2,3-d]pyrimidine (1 g, 3.56 mmol) and zinc dust (2.34 g, 35.6 mmol) were combined and stirred in ethanol (10 mL). NH4OH (1 mL) was added and the reaction heated to reflux for 2 hours. The reaction mixture was allowed to cool to room temperature, diluted with ethyl acetate (50 mL) and filtered through celite. The filtrate was washed with water (100 mL), dried over Na2SO4 and concentrated at reduced pressure. The resulting residue was purified by flash chromatography, eluting with a gradient of petroleum ether to 90/10 petroleum ether/ethyl acetate to afford 2-chloro-5-phenyl-thieno[2,3-d]pyrimidine (260 mg).

1. temperaturethe reaction heated
2. temperatureto reflux for 2 hours
3. filtrationfiltered through celite
4. washThe filtrate was washed with water (100 mL)
5. dry with materialdried over Na2SO4
6. concentrationconcentrated at reduced pressure
7. customThe resulting residue was purified by flash chromatography
8. washeluting with a gradient of petroleum ether to 90/10 petroleum ether/ethyl acetate