三（全氟苯基）对羟基苯基硼酸三乙铵的合成与单晶结构

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。

Synthesis and crystalline structure of triethylamonium tris(perfluorophenyl)-p-hydroxyphenylborate

Triethylammonium (p-hydroxyphenyl) tris (pentafluorophenyl) borate (a) was successfully synthesized by deprotection of triethylammenium (4-(tert-Butyldimethyl silanyloxyphenyl) tris(pentafluorophenyl) borate (b) in Et3N·3HF-THF solution, wherein (b) was obtained by reacting tris(pentafluorophenyl) borane with (4-((tert-butyldimethylsilyl) oxy) phenyl) magnesium bromide. Under the optimized reaction conditions, in which the molar ratio of 4-TBDMSO-C6H4MgBr/(C6F5)3B, NEt3∙HCl/B and NEt3∙3HF/B is 3:1, 5.7:1 and 1.3:1 respectively , the molar yield of (a) borate is 54.2% on the basis of tris(pentafluorophenyl) borane and 19F NMR purity is 99.2%. Furthermore, crystal of this compound was obtained for the first time and X-ray single crystal diffraction analysis revealed that the compound crystallizes in Orthorhombic, space group Pbca.