反应详情

温度

85 °C

A mixture of C6 (51 mg; 0.126 mmol) and 1:1 (vol:vol) t-BuOH/dichloroethane (500 μL) was added to a mixture of N-(3-Aminomethyl-pyridin-2-yl)-N-methyl-methanesulfonamide (38 mg, 0.139 mmol) and diisopropyl ethylamine (66 μL, 0.378 mmol). The reaction mixture was heated to 85° C. in a sealed vial. After two hours, the hot reaction mixture was loaded directly onto silica under reduced pressure, purified via chromatography (99:1:0.1 CHCl3:CH3OH:NH4OH), and concentrated under reduced pressure to provide 1 as a white solid (13 mg, 0.0223 mmol, 18%). LC/MS (Method F) r.t.=2.26 min.; m/z 583.2. HPLC r.t.=6.40 min.

1. custompurified via chromatography (99:1:0.1 CHCl3:CH3OH:NH4OH)
2. concentrationconcentrated under reduced pressure