反应详情

To an ice cooled solution of 5-bromo-2-chlorobenzoyl chloride in dichloromethane (35 mL) was added 1-(2,3-dihydro-benzo[1,4]oxazin-4-yl)-2,2,2-trifluoro-ethanone (6.5 g, 28.1 mmol) in dichloromethane (45 mL) followed by AlCl3 (5.61 g, 42.2 mmol) portion wise. After 2 h, the reaction mixture was brought to room temperature and stirred overnight. The reaction was quenched by pouring it over crushed ice. The resulting mixture was extracted with dichloromethane. The organic layer was washed with aq. NaHCO3 (100 mL) and water (100 mL), and the solvent was evaporated to yield the crude product which was recrystallized from hot ethylacetate to furnish 1-[6-(5-bromo-2-chloro-benzoyl)-2,3-dihydro-benzo[1,4]oxazin-4-yl]-2,2,2-trifluoro-ethanone (10.0 g).

1. customwas brought to room temperature
2. customThe reaction was quenched
3. additionby pouring it
4. customover crushed ice
5. extractionThe resulting mixture was extracted with dichloromethane
6. washThe organic layer was washed with aq. NaHCO3 (100 mL) and water (100 mL)
7. customthe solvent was evaporated
8. customto yield the crude product which
9. customwas recrystallized from hot ethylacetate