反应详情

温度

80 °C

Four batches of 6-chloro-3-pyridinecarbonitrile (0.40 g, 2.89 mmol) in methylamine (16 mL, 2M solution in THF) were each heated at 80° C. for 30 minutes in a microwave reactor. The reaction mixtures were combined and concentrated in vacuo. The residue was re-dissolved in EtOAc/water and the organic layer was separated, dried (Na2SO4) and concentrated. The crude product was purified by column chromatography; elution with EtOAc/petroleum ether gave the title compound as a white solid (1.46 g). δH (CDCl3, 400 MHz) 8.37 (1H, d), 7.59 (1H, dd), 6.39 (1H, dd), 5.19 (1H, br.s), 2.99 (3H, d). MS (ES): MH+ 134.2.

1. customThe reaction mixtures
2. concentrationconcentrated in vacuo
3. dissolutionThe residue was re-dissolved in EtOAc/water
4. customthe organic layer was separated
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated
7. customThe crude product was purified by column chromatography
8. washelution with EtOAc/petroleum ether