Hydrogen Bromide → Ethanone, 2,2-dibromo-1-(3-pyridinyl)-, hydrobromide
反応式
C(OC(=O)[CH2:5][C:6]([C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1)=[O:7])C.[BrH:15].[Br:16]Br>>[BrH:15].[Br:15][CH:5]([Br:16])[C:6]([C:8]1[CH:9]=[N:10][CH:11]=[CH:12][CH:13]=1)=[O:7]参加物
4
実験手順
3-(3-Pyridyl)-3-oxopropionic acid ethyl ester (1.95 g, 10.2 mmol) was added dropwise to 47% aqueous HBr solution (3.86 g) under ice-cooling. Bromine (2.2 g, 1.2 equivalent amount relative to 3-(3-pyridyl)-3-oxopropionic acid ethyl ester) was added dropwise at not more than 10° C. After stirring for 30 min, iced-water bath was removed and water (2 ml) and 47% aqueous HBr solution (4 ml) were added. The mixture was stirred at room temperature for 30 min. Furthermore, bromine (2.2 g, 1.2 equivalent amount relative to 3-(3-pyridyl)-3-oxopropionic acid ethyl ester) was added dropwise and the mixture was stirred at 65-70° C. After cooling to room temperature, the reaction mixture was filtrated to give 3.73 g of the titled compound (yield 95.2%).