反应详情

The unpurified 3-(3-bromo-4-fluoro-phenyl)-acryloyl chloride (3.5 g, 13.3 mmol) prepared in Step 2, N,O-dimethylhydroxylamine hydrochloride (1.4 g, 14.0 mmol), and pyridine (2.4 mL, 29.4 mmol) were added at 0° C. to dichloromethane (20.0 mL). The reaction mixture was stirred at room temperature for 12 hours, quenched with a 1N hydrochloric acid solution, and then extracted with diethyl ether two times. The combined extract was washed with a saturated solution of sodium hydrogen carbonate 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 3.2 g of the titled compound as a white solid.

1. customquenched with a 1N hydrochloric acid solution
2. extractionextracted with diethyl ether two times
3. extractionThe combined extract
4. washwas washed with a saturated solution of sodium hydrogen carbonate and brine
5. dry with materialdried on anhydrous magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customto give a yellow liquid residue
8. customThe resulting residue was recrystallized from diethyl ether and n-hexane