反应详情

While a solution of 2.43 g 5-bromo-2-fluorophenylamine (compound in Production Example 335), 2.6 g benzophenone and 122 mg 4-toluenesulfonic acid in 50 ml toluene was azeotropically dehydrated, the mixture was heated for 6 hours under reflux. The reaction mixture was diluted with ethyl acetate and washed with brine, the organic layer was dried over anhydrous sodium sulfate, the solvent was removed, and the resulting crude product was purified by silica gel column chromatography (ethyl acetate/hexane) to give 1.91 g of the title compound (colorless oil).

1. temperaturethe mixture was heated for 6 hours
2. temperatureunder reflux
3. washwashed with brine
4. dry with materialthe organic layer was dried over anhydrous sodium sulfate
5. customthe solvent was removed
6. customthe resulting crude product was purified by silica gel column chromatography (ethyl acetate/hexane)