反应详情

温度

50 °C

To a round bottom flask are added 5-(4-tert-butylamino-3-nitro-phenyl)-pyrimidin-2-ylamine (6.3 g, 0.02 mol) and ammonium formate (6.9 g, 0.1 mol) in EtOH, (100 mL), followed by the addition of zinc dust (4.3 g, 0.066 mol). The reaction mixture is stirred at 50° C. for 2 hours. The reaction mixture is filtered through a short pad of diatomaceous earth. The filter pad is rinsed with MeOH (50 mL) and the combined filtrate is concentrated. The residue is extracted with H2O (50 mL) and EtOAc (3×50 mL). The combined organic layer is washed with saturated NaHCO3 solution (30 mL), dried (MgSO4) and filtered. The filtrate is concentrated to afford 4-(2-amino-pyrimidin-5-yl)-N1-tert-butyl-benzene-1,2-diamine as a dark purple solid (4.5 g, 80%). LCMS (ESMS): m/z 258.20 (M++1)

1. filtrationThe reaction mixture is filtered through a short pad of diatomaceous earth
2. washThe filter pad is rinsed with MeOH (50 mL)
3. concentrationthe combined filtrate is concentrated
4. extractionThe residue is extracted with H2O (50 mL) and EtOAc (3×50 mL)
5. washThe combined organic layer is washed with saturated NaHCO3 solution (30 mL)
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. concentrationThe filtrate is concentrated