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制备实施例1 4-氟苯乙基溴的合成:在冰浴冷却条件下,将三苯基膦(222 g)和N-溴代琥珀酰亚胺(151 g)依次加入至4-氟苯乙醇(100 g)的二氯甲烷(1 L)溶液中,持续搅拌反应1小时。反应完成后,对所得溶液进行减压浓缩,随后过滤析出的晶体。进一步浓缩滤液,得到目标产物4-氟溴乙基苯(133 g),为无色油状物(收率:92%)。产物经1H-NMR(400 MHz,CDCl3)表征:δ(ppm)3.14(2H,t,J = 8 Hz),3.54(2H,t,J = 8 Hz),6.98-7.03(2H,m),7.15-7.18(2H,m)。
参考文献:
[1] Journal of Organic Chemistry, 2006, vol. 71, # 18, p. 7035 - 7044
[2] Tetrahedron Asymmetry, 2001, vol. 12, # 4, p. 585 - 596
[3] Patent: US2002/19531, 2002, A1
[4] Bioorganic and Medicinal Chemistry, 2009, vol. 17, # 8, p. 2989 - 3002
[5] Patent: EP2508526, 2012, A1. Location in patent: Page/Page column 48