反应详情

温度

90 °C

[2-(4-Acetamido-phenylsulfanyl)-7-nitroquinazolin-4-yl]-(5-methyl-2H-pyrazol-3-yl)-amine (182 mg, 4.18.10−4 mol) is dissolved in a mixture EtOH/water/AcOH(25/10/1, 36 mL) and the reaction is heated at 90° C. Iron powder (93 mg) is added and the mixture is stirred at 90° C. for 4 hours, cooled to room temperature and filtered through a pad of celite. The pad is washed with methanol and the combined filtrate is concentrated in vacuo. The residue is purified by flash chromatography (SiO2, DCM/MeOH gradient) to give the desired [2-(4-acetamido-phenylsulfanyl)-7-aminoquinazolin-4-yl]-(5-methyl-2H-pyrazol-3-yl)-amine.

1. temperaturecooled to room temperature
2. filtrationfiltered through a pad of celite
3. washThe pad is washed with methanol
4. concentrationthe combined filtrate is concentrated in vacuo
5. customThe residue is purified by flash chromatography (SiO2, DCM/MeOH gradient)