10531-41-6

88-15-3

10531-41-6

实施例1.12：2-溴-1-（噻吩-2-基）乙-1-酮的合成。将溴（2.53 g，0.82 mL，0.0158 mol）的二氯甲烷（8 mL）溶液逐滴加入到2-乙酰噻吩（2.0 g，1.71 mL，0.0158 mol）的二氯甲烷（10 mL）溶液中。反应混合物在25℃下搅拌1小时，随后用饱和碳酸氢钠水溶液中和。有机层用水洗涤并干燥。溶剂蒸发后，通过柱色谱（硅胶，洗脱剂为乙酸乙酯:正己烷=5:95）纯化固体残余物，得到2-溴-1-（噻吩-2-基）乙-1-酮，为油状物（2.60 g，收率80%）。[注：1-（噻吩-2-基）乙-1-酮的替代制备方法近期已有报道，参见：Ostrowski, T.; Golankiewicz, B.; De Clercq, E.; Andrei, G.; Snoeck, R. Synthesis and anti-VZV activity of tricyclic acyclovir and 9-{[cis-1',2'-bis(hydroxymethyl)cycloprop-1'-yl]methyl}guanine analogues as 6-heteroaryl derivatives. Eur. J. Med. Chem. 2009, 44, 3313-3317.]

参考文献：

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[4] ChemMedChem, 2018, vol. 13, # 11, p. 1102 - 1114

[5] Phosphorus, Sulfur and Silicon and the Related Elements, 2013, vol. 188, # 12, p. 1835 - 1844