反应详情

温度

100 °C

To a suspension of tert-butyl 5-((2,5-dichloropyrimidin-4-yl)amino)hexahydrocyclopenta[c]pyrrole-2(1H)-carboxylate (579.1 mg, 1.55 mmol) and 1,5-dimethylpyrazol-4-amine hydrochloride (446.8 mg, 3.03 mmol) in dioxane (10 mL) was added trifluoroacetic acid (862.8 mg, 7.57 mmol). The reaction mixture was stirred at 100° C. overnight and adjusted to pH=10 with a saturated Na2CO3 solution, then extracted with DCM (100 mL×3). The combined organic phases were washed with brine (100 mL), dried over anhydrous Na2SO4, filtered and concentrated in vacuo. The residue was purified by silica gel column chromatography (MeOH/DCM=1/10) to give the title compound as a beige solid (105.6 mg, 19.6%).

1. extractionextracted with DCM (100 mL×3)
2. washThe combined organic phases were washed with brine (100 mL)
3. dry with materialdried over anhydrous Na2SO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe residue was purified by silica gel column chromatography (MeOH/DCM=1/10)