反应详情

To a solution of quinolin-5-yl-methylamine 100 mg, 0.39 mmol) and diisopropylethylamine (140 μL, 0.78 mmol) in a mixture of DMF (2 mL) and acetonitrile (2 mL) was added {4-[(2-chloro-5-nitro-pyrimidin-4-ylamino)-methyl]-cyclohexyl}-carbamic acid tert-butyl ester (150 mg, 0.39 mmol). The reaction mixture was stirred at room temperature for 16 h. The reaction mixture was diluted with ethyl acetate and washed with water (×2). The combined organic phase was dried over Na2SO4 and concentrated. The resulting residue was purified by silica gel prep TLC using 95:5 CH2Cl2:MeOH as an eluent to afford 197 mg of [4-({5-nitro-2-[(quinolin-5-ylmethyl)-amino]-pyrimidin-4-ylamino}-methyl)-cyclohexyl]-carbamic acid tert-butyl ester as a light yellow solid (100%).

1. washwashed with water (×2)
2. dry with materialThe combined organic phase was dried over Na2SO4
3. concentrationconcentrated
4. customThe resulting residue was purified by silica gel prep TLC