9,9-双(甲氧基甲基)芴的合成及其结构表征

在四丁基溴化铵相转移催化剂的作用下,以甲苯为溶剂,9,9-双羟甲基芴(BHMF)、NaOH、碳酸二甲酯为原料,通过烷基化反应合成了新型给电子体9,9-双(甲氧基甲基)芴(BMMF);考察了原料配比、催化剂的种类及用量、碳酸二甲酯的用量、反应温度等因素对BMMF收率的影响;采用红外光谱和核磁共振光谱对产物结构进行了表征。实验结果表明,合成BMMF的最佳工艺条件为:0.1mol BHMF,n(BHMF)∶n(NaOH)∶n(碳酸二甲酯)=1.0∶10.0∶2.2,催化剂四丁基溴化铵1.25g,反应温度20℃,甲苯溶剂240mL。在此条件下,BMMF的收率达69.1%,产品纯度为99.3%。

Synthesis and Characterization of 9,9-Bis (Methoxymethyl) Fluorene

9,9-Bis(methoxymethyl) fluorene(BMMF),a new type of electron donor for Ziegler-Natta polypropylene catalysts,was synthesized from 9,9-bis(hydroxymethyl)fluorene(BHMF),NaOH and dimethyl carbonate with tetrabutylammonium bromide(TBAB)as phase transfer catalyst.The prepared BMMF was characterized by means of IR and NMR,and its purity was analyzed by GC.Effects of n(BHMF) ∶n(NaOH) ∶n(dimethyl carbonate),different phase transfer catalysts,TBAB catalyst dosage,dimethyl carbonate dosage and reaction temperature on yield of BMMF were investigated.Under optimal reaction conditions: BHMF 0.1 mol,n(BHMF) ∶n(NaOH) ∶n(dimethyl carbonate) 1.0 ∶10.0 ∶2.2,TBAB dosage 1.25 g,reaction temperature 20 ℃ and solvent toluene dosage 240 mL,yield of BMMF is 69.1% and its mass fraction in the products is 99.3%.