反应详情

A solution of 4-(2-amino-pyrimidin-5-yl)-N1-tert-butyl-benzene-1,2-diamine (180 mg, 0.70 mmol) and 2-(4-methyl-pyrazol-1-yl)-benzaldehyde (130 mg, 0.70 mmol) in acetic acid (5 mL) is warmed to 100° C. for 16 hours then cooled to room temperature and neutralized with NaHCO3 (sat.). The product is extracted into EtOAc (3×) and the combined organics are dried (MgSO4), filtered and concentrated. Purification via flash chromatography (12 g silica gel, 0-5% MeOH/CH2Cl2) affords the title compound (105 mg, 35%). LCMS (ESMS): m/z 424.20 (M++1)

1. extractionThe product is extracted into EtOAc (3×)
2. dry with materialthe combined organics are dried (MgSO4)
3. filtrationfiltered
4. concentrationconcentrated
5. customPurification via flash chromatography (12 g silica gel, 0-5% MeOH/CH2Cl2)