反应详情

温度

50 °C

To a solution of 1-(6-benzyl-4,5-dimethyl-pyridazin-3-yl)-piperidine-4-carboxylic acid cyanomethyl-amide (20 mg, 0.055 mmol) and triphenyl phosphine in acetonitrile (1 mL) at 25° C. is added carbon tetrachloride (42 mg, 0.28 mmol). After being stirred at 50° C. for 3 h, the mixture is concentrated, and diluted with CH2Cl2 (10 mL) and washed with sodium hydroxide (2 mL, 1N), and H2O (2 mL), dried over Na2SO4, filtered and concentrated. The crude product is purified by HPLC (CH3CN/H2O: 22%˜45% with 0.1% TFA) to give 3-benzyl-6-[4-(5-chloro-1H-imidazol-2-yl)-piperidin-1-yl]-4,5-dimethyl-pyridazine (11.8 mg, 56%).

1. concentrationthe mixture is concentrated
2. additiondiluted with CH2Cl2 (10 mL)
3. washwashed with sodium hydroxide (2 mL, 1N), and H2O (2 mL)
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude product is purified by HPLC (CH3CN/H2O: 22%˜45% with 0.1% TFA)