反应详情

Dissolve {2-[4-(3-carbamoylpyridin-2-yloxy)phenyl]ethyl}carbamic acid tert-butyl ester (0.518 g, 1.45 mmol) in dichloromethane (8.4 mL). Add TFA (8.4 mL) and stir at room temperature for 4 hours. Concentrate the reaction mixture. Load the product onto an SCX column with methanol. Wash the column with methanol then elute with 50% (2.0 M NH3 in methanol) in methanol to give the title compound (0.38 g, 100%): TOF MS ES+ 258.1 (M+H)+, base peak TOF ES+ 241.1 (M-NH2)+, HRMS calcd for C14H16N3O2 258.1243 (M+H)+, found 258.1228, time 0.34 min; HPLC [YMC-Pack Pro C-18 (150×4.6 mm, S-5 microm), acetonitrile in water containing 0.01% concentrated HCl at 1.0 mL/min, 5-95% over 19 min], tR=13.4 min, 100% purity.

1. concentrationConcentrate the reaction mixture
2. washWash the column with methanol
3. washthen elute with 50% (2.0 M NH3 in methanol) in methanol