反应详情

To a solution of 4-bromo-2-chloro-5-trifluoromethoxy-phenylamine (0.55 g, 1.90 mmol) in DCM (4.9 mL) was added CDI (0.34 g, 2.09 mmol). The reaction solution was stirred at RT overnight and then 4-piperazin-1-yl-piperidine-1-carboxylic acid tert-butyl ester (0.56 g, 2.09 mmol; Preparation 12) was added and the reaction mixture was stirred for 30 min at RT, concentrated under vacuum and purified by silica gel chromatography (0-5% MeOH/DCM). Pure fractions were combined and concentrated under vacuum to provide the title intermediate (0.67 g, 60% yield) as a white foam. (m/z): [M+H]+ calcd for C22H29BrClF3N4O4 585.1 found 584.6.

1. stirringthe reaction mixture was stirred for 30 min at RT
2. concentrationconcentrated under vacuum
3. custompurified by silica gel chromatography (0-5% MeOH/DCM)
4. concentrationconcentrated under vacuum