反应详情

温度

80 °C

A mixture of [5-({[1-(4-Chloromethyl-benzyl)-1H-pyrazole-4-carbonyl]-amino}-methyl)-4,6-dimethyl-pyridin-2-yl]-carbamic acid tert-butyl ester (67 mg, 0.1 mmol), succinimide (12 mg, 0.1 mmol) and potassium carbonate (84 mg, 0.6 mmol) in 50 mL acetone was stirred at 80° C. for 24 h. The mixture was filtrated and concentrated in vacuo. The crude was purified by preparative HPLC (Waters Sunfire Prep C18 PBD 5 um, 30×100 mm, 5 to 100% ACN and 0.1% TFA, flow 40ml/min) to yield the title compound. LCMS (method A) RtA=1.339 min; [M+H]+=547.2.

1. filtrationThe mixture was filtrated
2. concentrationconcentrated in vacuo
3. customThe crude was purified by preparative HPLC (Waters Sunfire Prep C18 PBD 5 um, 30×100 mm, 5 to 100% ACN and 0.1% TFA, flow 40ml/min)