反应详情

To a solution of 4-(2-amino-pyrimidin-5-yl)-N1-tert-butyl-benzene-1,2-diamine (100 mg, 0.39 mmol) in DMF (5 mL) is added 2-(2,4-dimethyl-thiazol-5-yl)-5-methoxy-benzaldehyde (144 mg, 0.58 mmol) at room temperature. Oxone (239 mg, 0.39 mmol) in H2O (1 mL) is added and the solution is stirred for 4 hours. Saturated sodium thiosulfate solution (5 mL) is added and the mixture is extracted with EtOAc (3×10 mL) and H2O (10 mL). The combined organic layer is dried with MgSO4 and is filtered. The filtrate is concentrated and the residue is purified by silica gel flash column chromatography eluting with 10% MeOH in CH2Cl2 to afford the title compound (81 mg, 43%) as a pale brown foam. LCMS (ESMS): m/z 485.72 (M++1)

1. extractionthe mixture is extracted with EtOAc (3×10 mL) and H2O (10 mL)
2. dry with materialThe combined organic layer is dried with MgSO4
3. filtrationis filtered
4. concentrationThe filtrate is concentrated
5. customthe residue is purified by silica gel flash column chromatography
6. washeluting with 10% MeOH in CH2Cl2