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温度

0 °C

To (2-aminomethyl-quinazolin-4-yl)-(4-methoxy-phenyl)-methyl-amine (100 mg, 0.34 mmol) and nicotinoyl chloride hydrochloride (91 mg, 0.51 mmol) in CH2Cl2 (3 mL) at 0° C. was added triethylamine (167 mg, 1.2 mmol). The reaction was stirred for 2 h at 0° C. The mixture was washed successively with H2O, 0.1 M HCl, H2O and 5% NaHCO3. The reaction was extracted with EtOAc (3×10 mL), washed with brine, dried (MgSO4) and concentrated providing 64 mg of the title compound. 1H NMR (CDCl3) δ 8.76 (s, 1H), 8.29 (d, 1H), 8.11 (s, 1H), 7.78 (d, 1H), 7.58 (t, 1H), 7.45 (t, 1H), 7.14 (d, 2H), 7.05-7.01 (m, 2), 6.93 (d, 2H), 4.85 (s, 2H), 3.85 (s, 3H), 3.61 (s, 3H); LC-MS (ESI+; 400 ([M+H]+)).

1. washThe mixture was washed successively with H2O, 0.1 M HCl, H2O and 5% NaHCO3
2. extractionThe reaction was extracted with EtOAc (3×10 mL)
3. washwashed with brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated