反应详情

温度

160 °C

To a solution of 6-chloro-pyridine-3-sulfonic acid (4-fluoro-phenyl)-isobutyl-amide (150 mg, 439 μmol) and 4-amino-1-boc piperidine (114 mg, 570 μmol) in acetonitrile (3 mL) was added DIPEA (115 μl, 658 μmol) and the reaction was heated at 160° C. in a microwave reactor for 2.5 hours. EtOAc and saturated aqueous NaHCO3 were added, extracted, washed with brine, dried with Na2SO4 then concentrated and purified by silica gel column chromatography (0-50% EtOAc in cyclohexane) to give 4-{5-[(4-fluoro-phenyl)-isobutyl-sulfamoyl]-pyridin-2-ylamino}-piperidine-1-carboxylic acid tert-butyl ester (69 mg, 31%). LCMS (m/z, Method A) ES− 506 [M−1]−.

1. extractionextracted
2. washwashed with brine
3. dry with materialdried with Na2SO4
4. concentrationthen concentrated
5. custompurified by silica gel column chromatography (0-50% EtOAc in cyclohexane)