反应详情

温度

105 °C

A mixture of [1-(4-azidopyridin-3-yl)meth-(E)-ylidene]-(2.6-dichloro-4-methanesulfonylphenyl)amine (4.21 mmol) in toluene (15 mL) was heated to 105° C. for 18 hours. The reaction mixture was allowed to cool and then concentrated under reduced pressure. The residue was recrystallised from ethyl acetate and the solid was collected by filtration to afford the title compound as a beige solid (0.75 g, 52% yield). 1H NMR (300 MHz, DMSO-d6): δ 9.38 (d, J=1.4 Hz, 1H) 9.15 (d, J=1.0 Hz, 1H), 8.34 (s, 2H) 8.31 (d, J=6.4 Hz, 1H) 7.68 (dt, J=6.4, 1.2 Hz, 1H) 3.49 (s, 3H). LCMS (Method D): RT=1.72 min, m/z: 342 [M+H+].

1. temperatureto cool
2. concentrationconcentrated under reduced pressure
3. customThe residue was recrystallised from ethyl acetate
4. filtrationthe solid was collected by filtration