反应详情

To a solution of 1-N-[3-fluoro-5-(trifluoromethyl)pyridin-2-yl]-1-methylcyclopentane-1,2-diamine (Intermediate 28; 0.225 g, 0.81 mmol) and 4-methylmorpholine (0.134 ml, 1.217 mmol) in acetonitrile (5 ml) was added TOTU (0.399 g, 1.23 mmol) and 3-(pyrimidin-2-yl)pyridine-2-carboxylic acid (CAS number 1228431-21-7; 0.163 g, 0.81 mmol). The reaction was stirred at room temperature for 1 hour and then was diluted with DCM and washed with brine. The organics were dried over magnesium sulfate, concentrated in vacuo and purified by SCX chromatography (2M ammonia in methanol). The resulting residue was purified by column chromatography (silica, 0-10% methanol/DCM) and further purified by reverse phase chromatography (C18 silica, 5-95% water (0.05% ammonia)/acetonitrile) to afford the title compound.

1. washwashed with brine
2. dry with materialThe organics were dried over magnesium sulfate
3. concentrationconcentrated in vacuo
4. custompurified by SCX chromatography (2M ammonia in methanol)
5. customThe resulting residue was purified by column chromatography (silica, 0-10% methanol/DCM)
6. customfurther purified by reverse phase chromatography (C18 silica, 5-95% water (0.05% ammonia)/acetonitrile)