反应详情

1-(3,5-Dichloro-benzyl)-1H-imidazol-2-ylamine (see Example 12) was dissolved in anhydrous DMF and NaH was added to the solution under H2. The reaction mixture was stirred at room temperature for 10 min and 3-methoxybenzylbromide was added. The reaction mixture was stirred at 65° C. for 5 h. The reaction mixture was then diluted with EtOAc and washed with water (×5). The organic phase was dried over Na2SO4 and concentrated. The resulting residue was purified by silica gel preparative TLC using CH2Cl2:MeOH 95:5 to afford the title compound (7 mg, 5%); LCMS m/z 362 [C18H17Cl2N3O+H]+.

1. stirringThe reaction mixture was stirred at 65° C. for 5 h
2. washwashed with water (×5)
3. dry with materialThe organic phase was dried over Na2SO4
4. concentrationconcentrated
5. customThe resulting residue was purified by silica gel preparative TLC