Study On A New Process For Synthesis Of Bisphenol AF

In this paper Bisphenol AF was prepared in a new route which from HFA·3H₂O and aniline in 4 steps:alkylation,diazotization,hydrolysis,Friedel-Crafts alkylation,t he total yield was 67.4%.The produces were identified by GC/MS,IR and ¹H-NMR, and their reaction mechanism were discussed.The results are introduced as follows.(1)The synthesis of 2-(4-aminophenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol(â… ) was studied,which catalyzed by kinds of bronsted acids,the PEG ionic liquid and Nb₂O₅.The result showed that compound(â… ) was obtained with 96.3%yield under optimal conditions that Nb₂O₅ as the catalyst,n(HFA·3H₂O):n(aniline):n(Nb₂O₅) is 2:1:0.1,reflux condition and the reaction time is 6 h.The reaction mechanism is described as follows,because of oxygen vacancies,Nb₂O₅ is easy to accept the external electronics and form Lewis acid centers,which has good catalytic ability.(2)Then 2-(4-hydroxy phenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol(â…¡) was synthesize d from compound(â… ) via diazotization,hydrolysis.The optimum reaction conditions were as follows:during diazotization,n(â… ):n(H₂SO₄):n(NaNO₂) is 1:4.1:1.1,th e content of H₂SO₄ is 30%and reaction temperature- 2～2℃;during hydrolysis,the content of H₂SO₄ is 50%,n(H₂SO₄):n(â… ) is 11:1.Under these conditions,the yie ld was 89.4%.(3)In the presence of catalysts,the Friedel-Crafts alkylation of compound(â…¡) wh ich with phenol yielded target compound bisphenol AF(â…¢) was studied.The result s howed that methanesulfonic acid is the best catalyst,and Bisphenol AF was obtained with 78.3%yield.