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.