反应详情

5.3 g (18 mmol) of 4-bromo-N-(2-hydroxyphenyl)benzamide, 8.0 g (46 mmol) of para-toluenesulfonic acid monohydrate, and 200 mL of toluene were put in a 300 mL three-neck flask. This mixture was refluxed for four hours under a nitrogen atmosphere. Then, water was added to the mixture, and an organic layer and an aqueous layer were separated. An organic substance was extracted with ethyl acetate from the aqueous layer. The resulting extracted solution was combined with the organic layer, and the organic layer was washed with a saturated aqueous solution of sodium bicarbonate and then brine, and dried with magnesium sulfate. The obtained mixture was subjected to suction filtration through Celite (manufactured by Wako Pure Chemical Industries, Ltd., Catalog No. 531-16855), and the filtrate was concentrated to give a solid. The obtained solid was recrystallized with ethyl acetate/hexane, whereby 3.1 g of the target white powder was obtained in a yield of 61%.

1. temperatureThis mixture was refluxed for four hours under a nitrogen atmosphere
2. customan organic layer and an aqueous layer were separated
3. extractionAn organic substance was extracted with ethyl acetate from the aqueous layer
4. extractionThe resulting extracted solution
5. washthe organic layer was washed with a saturated aqueous solution of sodium bicarbonate
6. dry with materialbrine, and dried with magnesium sulfate
7. filtrationThe obtained mixture was subjected to suction filtration through Celite (manufactured by Wako Pure Chemical Industries, Ltd., Catalog No. 531-16855)
8. concentrationthe filtrate was concentrated
9. customto give a solid
10. customThe obtained solid was recrystallized with ethyl acetate/hexane