反应详情

A solution of 1-acetamido-7-pyrrolidin-1-yl-5,6,7,8-tetrahydronaphthalene (0.36 g, 1.4 mmol) and sodium acetate trihydrate (0.38 g, 2.8 mmol) in acetic acid (15 mL) was treated with bromine (0.27 g, 1.7 mmol) and stirred at room temperature for 2 h. A precipitate was collected by filtration and the filtrate evaporated. The two solids were combined and dissolved in methylene chloride; water. The mixture was basified with 12.5% NaOH, and the organic phase separated. The aqueous layer was back extracted and the combined organic layers were dried over sodium sulfate, filtered and evaporated. The residue was heated in diethyl ether to form a solid, which was collected and dried (0.31 g).

1. filtrationA precipitate was collected by filtration
2. customthe filtrate evaporated
3. dissolutiondissolved in methylene chloride
4. customthe organic phase separated
5. extractionThe aqueous layer was back extracted
6. dry with materialthe combined organic layers were dried over sodium sulfate
7. filtrationfiltered
8. customevaporated
9. temperatureThe residue was heated in diethyl ether
10. customto form a solid, which
11. customwas collected
12. customdried (0.31 g)