摘要
以山梨醇、苯甲醛为原料,在催化剂、助催化剂、脱水剂作用下,于常温反应合成了二亚苄叉山梨醇(DBS)。采用红外和核磁确认了DBS结构,考察了反应物配比、催化剂、助溶剂、助催化剂、吸水剂、反应时间和温度等因素对产品收率的影响。结果表明:n(山梨醇)∶n(苯甲醛)=1.0∶2.0,以浓硫酸、对甲苯磺酸和磷钨酸为催化剂,在二甲基亚砜和甲醇中室温反应3 h时,产品收率为95.9%,纯度98.2%。
Taking sorbitol and benzaldehyde as raw materials with the aid of catalysts, co-catalysts, and dehydrating agents, dibenzylidene sorbitol(DBS) was synthesized at room temperature. The structure of DBS was confirmed by IR and NMR, and the influence of factors including reactant ratio, catalyst, cosolvent, cocatalyst, water absorbent,reaction time and temperature on the product yield was investigated. The results showed that : n( sorbitol) ∶n(benzaldehyde) =1.0 ∶2.0, using concentrated sulfuric acid, p-toluenesulfonic acid and phosphotungstic acid as catalysts, reacting in dimethyl sulfoxide and methanol at room temperature for 3 h, the product yield was 95.9% with a purity of 98.2%.
作者
吴恩慧
张燕
许芸晗
王海蝶
李金洋
管西栋
WU En-hui;ZHANG Yan;XU Yun-han;WANG Hai-die;LI Jin-yang;GUAN Xi-dong(School of Pharmaceutical Sciences,Shandong First Medical University&Shandong Academy of Medical Scicenes,Taian 271016,China)
出处
《精细化工中间体》
CAS
2020年第5期57-60,共4页
Fine Chemical Intermediates
基金
国家级大学生创新创业训练计划(201910439002)
泰安市科技发展计划引导项目(2017GX0067)。