氯化镁催化苯酚一步法合成水杨醛

Synthesis of Salicylaldehyde by Catalysizing Phenol with Magnesium Chloride in an One-step Process

以苯酚为原料,氯化镁作催化剂,采用一步法合成了水杨醛,并用FT-IR及1HNMR对产品进行了结构表征。考察了催化剂、溶剂、缚酸剂、温度、反应时间及原料配比对产品收率、原料转化率的影响,得出适宜的合成条件为:0.01 mol苯酚,反应时间3 h,n(苯酚)∶n(氯化镁)∶n(三乙胺)∶n(多聚甲醛)=1∶3∶4∶7,温度为80℃,50 mL乙腈。此条件下,苯酚转化率为100%,水杨醛收率(以苯酚计)达80%。

The structure of salicylaldehyde,which was synthesized with phenol as the material and magnesium chloride as the catalyst in a one-step process,was characterized by FT-IR and 1H NHR techniques.The effects of catalyst,solvent,acid-binding agent,reaction temperature,reaction time and materials ratio on product yield and material conversion were studied,and appropriate synthesis conditions were identified: phenol amount: 0.01 mol,reaction time: 3 h,n(phenol) : n(magnesium chloride) : n(triethylamine) : n(paraformaldehyde) = 1: 3: 4: 7,reaction temperature: 80 ℃,amount of acetonitrile solvent: 50 mL.The conversion of phenol was 100%,and the yield of salicylaldehyde(in terms of phenol) was 80% at such conditions.