反应详情

温度

100 °C

To a solution of (4-bromo-2-nitro-phenyl)-tert-butyl-amine (7.2 g, 0.026 mol) in DMF (100 mL) and H2O (10 mL) are added 5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-pyrimidin-2-ylamine (8.7 g, 0.04 mol), Pd(PPh3)4 (3 g, 0.003 mol) and K2CO3 (7.3 g, 0.053 mol) at room temperature. The solution is heated to 100° C. for 2 hours. The solution is cooled down, washed with H2O (100 mL) and extracted with EtOAc (3×50 mL). The combined organic layer is dried with MgSO4 and filtered. The filtrate is concentrated and the residue is re-crystallized in CH2Cl2 (10 mL) to afford 5-(4-tert-butylamino-3-nitro-phenyl)-pyrimidin-2-ylamine as a scarlet solid (6.3 g, 83%).

1. temperatureThe solution is cooled down
2. washwashed with H2O (100 mL)
3. extractionextracted with EtOAc (3×50 mL)
4. dry with materialThe combined organic layer is dried with MgSO4
5. filtrationfiltered
6. concentrationThe filtrate is concentrated
7. customthe residue is re-crystallized in CH2Cl2 (10 mL)