反应详情

In a 300 mL three-neck flask, 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 placed. This mixture was stirred for 4 hours under nitrogen stream. After a certain period, water was added to the mixture, and an aqueous layer was extracted with ethyl acetate. The resulting extracted solution and the organic layer were combined and washed with a saturated aqueous solution of sodium hydrogen carbonate and saturated saline, and then the organic layer was dried with magnesium sulfate. The mixture obtained was subjected to suction filtration through Celite (produced by Wako Pure Chemical Industries, Ltd., Catalog No. 531-16855), and the filtrate was condensed to give a solid. The solid was recrystallized with ethyl acetate/hexane, so that 3.1 g of target white powder was obtained in a yield of 61%.

1. waitAfter a certain period
2. extractionan aqueous layer was extracted with ethyl acetate
3. extractionThe resulting extracted solution
4. washwashed with a saturated aqueous solution of sodium hydrogen carbonate and saturated saline
5. dry with materialthe organic layer was dried with magnesium sulfate
6. customThe mixture obtained
7. filtrationwas subjected to suction filtration through Celite (produced by Wako Pure Chemical Industries, Ltd., Catalog No. 531-16855)
8. customcondensed
9. customto give a solid
10. customThe solid was recrystallized with ethyl acetate/hexane, so that 3.1 g of target white powder
11. customwas obtained in a yield of 61%