反应详情

3-[3-(4-Cyano-phenyl)-ureidomethyl]-benzoic acid (30 mg, 0.1 mmol), prepared as described in Example 1, EDC (28.8 mg, 0.15 mmol), and HOBt (17.6 mg, 0.13 mmol) were combined in a reaction vial and DMF (1 mL) then N-methylmorpholine (0.017 mL, 0.15 mmol) were added. The reaction mixture was agitated for 30 minutes, then N1,N1-dimethyl-butane-1,4-diamine (14 mg, 0.12 mmol) was added. Shaking was continued overnight. The reaction mixture was purified by preparative HPLC using an acetonitrile/water/formic acid gradient. The title compound was collected as a formate salt (36 mg, 90% yield) following evaporation of the solvent; MS analysis electrospray, 394 (M+H).

1. stirringShaking
2. waitwas continued overnight
3. customThe reaction mixture was purified by preparative HPLC