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采用三(五氟苯基)硼烷与4-[叔丁基二(甲基)硅氧基]苯基溴化镁格氏试剂反应,再经三乙胺三氢氟酸-四氢呋喃溶液反应脱除保护基,得到(对羟基苯基)三(五氟苯基)硼酸三乙铵(a),在n(4-TBDMSO-C6H4MgBr)/n〔(C6F5)3B〕、n(NEt3.HCl)/n〔(C6F5)3B〕、n(NEt3.3HF)/n〔(C6F5)3B〕分别为3∶1、5.7∶1、1.3∶1的工艺条件下,所得产品质量分数达99.2%,基于三(五氟苯基)硼烷的收率达54.2%,并首次得到该化合物的单晶,X射线单晶结构分析表明,该化合物属正交晶系,Pbca空间群。
The reaction was carried out with tris (pentafluorophenyl) borane and 4- [tert-butyldimethylsiloxy] phenylmagnesium bromide Grignard reagent, followed by triethylamine trihydrofluoride-tetrahydrofuran solution (4-TBDMSO-C6H4MgBr) / n [(C6F5) 3B], n (NEt3.HCl) is obtained by removing the protective group to give triethylammonium (p- hydroxyphenyl) /nwe(C6F5)3Balln, (NEt3.3HF) / nwe (C6F5) 3B] were 3: 1, 5.7: 1, 1.3: 1 under the process conditions, the resulting product mass fraction of 99.2%, based on The yield of tris (pentafluorophenyl) borane reached 54.2%, and the single crystal of the compound was obtained for the first time. The X-ray single crystal structure analysis showed that the compound belongs to orthorhombic Pbca space group.