反应详情

The 3-(5-bromo-pyridin-3-yl)-acryloyl chloride in the form of unpurified dark brown liquid, N,O-dimethylhydroxylamine hydrochloride (11.6 g, 119.3 mmol), and pyridine (20.4 mL, 252.4 mmol) were added at 0° C. to dichloromethane (150.0 mL). The reaction mixture was stirred at room temperature for 3 hours, quenched with distilled water, and then extracted with dichloromethane. The extract was washed with a 1N hydrochloric acid solution and brine, dried on anhydrous magnesium sulfate, and then concentrated under reduced pressure to give a yellow liquid residue. The resulting residue was recrystallized from diethyl ether and n-hexane to give 8.2 g of the titled compound as a yellow solid.

1. customquenched with distilled water
2. extractionextracted with dichloromethane
3. washThe extract was washed with a 1N hydrochloric acid solution and brine
4. dry with materialdried on anhydrous magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. customto give a yellow liquid residue
7. customThe resulting residue was recrystallized from diethyl ether and n-hexane