Ammonium formate → 4-(2-amino-pyrimidin-5-yl)-N1-tert-butyl-benzene-1,2-diamine

関与物質

反応条件

反応手順

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)

情報源と証拠