反应详情

To a solution of 4-(2-amino-pyrimidin-5-yl)-N1-tert-butyl-benzene-1,2-diamine (50 mg, 0.194 mmol) in DMF (10 mL) is added 5-methoxy-2-1,2,4-triazol-1-yl-benzaldehyde (47 mg, 0.233 mmol) at room temperature. Oxone (119 mg, 0.194 mmol) in H2O (2 mL) is added and the solution is stirred for 1 hour. 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, filtered and concentrated. The residue is purified by silica gel flash column chromatography eluting with 10% MeOH in CH2Cl2 to afford the title compound (41 mg, 47%) as a pale brown solid. LCMS (ESMS): m/z 441.20 (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. filtrationfiltered
4. concentrationconcentrated
5. customThe residue is purified by silica gel flash column chromatography
6. washeluting with 10% MeOH in CH2Cl2