反应详情

To a round bottom flask is added 4-(2-amino-4-methoxy-pyrimidin-5-yl)-N1-tert-butyl-benzene-1,2-diamine (118 mg, 0.411 mmol) in DMF (4 mL) and water (1 mL), followed by the addition of 2-1,2,4-triazol-1-yl-benzaldehyde (78 mg, 0.45 mmol) and oxone (51 mg, 0.443 mmol). The reaction mixture is stirred at room temperature for 4 hours. Sat. sodium thiosulfate (10 mL) is added. The reaction mixture is diluted with EtOAc. The organic layer is separated, washed with water then brine, dried with Na2SO4, filtered and concentrated. The residue is loaded into a silica gel column. The column is eluted with 0-4% 7M NH3 in MeOH/CH2Cl2. The product fractions are collected and concentrated to afford the title compound (67 mg, 37%) as a light brown solid. LCMS (ESMS): m/z 441.73 (M++1)

1. customThe organic layer is separated
2. washwashed with water
3. dry with materialbrine, dried with Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. washThe column is eluted with 0-4% 7M NH3 in MeOH/CH2Cl2
7. customThe product fractions are collected
8. concentrationconcentrated