糠偶酰的制备

A novel synthesis of furil

研究了一种以糠醛为原料,盐酸硫胺素(VB1)为催化剂,在碱性条件,pH=8～9,采用安息香缩合反应合成中间体糠偶姻,并利用硫酸铜-吡啶氧化其为糠偶酰。实验考查了反应温度、反应时间、催化剂用量、氧化剂用量对中间体或产品收率的影响,确定合成工艺的最佳条件为:中间体反应温度65℃,反应时间2.0h,催化剂m(VB1)=8.0g,最高收率82.7%;产品反应温度100℃,反应时间2.5h,n(硫酸铜)∶n(吡啶)∶n(水)=1∶4.3∶9.0,最高收率91.7%。中间体为白色针状晶体,熔点为138～139℃。产品为黄色针状晶体,熔点为165～166℃。产物结构用红外光谱、元素分析方法进行表征。

Preparation of furoin using furfural as raw materials and VB1 as catalysis has been studied in alkaline conditions,pH of 8 to 9.Furoin was oxidized to furil by CuSO4-C5H5N as an oxidant.The effect of reaction temperature,reaction time,the amount of VB1 and oxidant.on the yield of the product was observed.Optimum conditions of synthesizing technology of furoin were determined,reaction temperature was 65 ℃,the mixture was refluxed for 2 hours,the amount of VB1 was 8.0 g.The yield of the product reached 82.7%.Optimum conditions of synthesizing technology of furil were determined,reaction temperature was 100 ℃,the mixture was refluxed for 2.5 hours,n（CuSO4）：n（C5H5N）∶n（H2O） = 1∶4.3∶9.0.The yield of the product reached 91.7%.The product of furoin is white needle-like crystals,the melting point of 138~139 ℃.The product of furil is yellow needle-like crystals,the melting point of 165~166 ℃.Structure of objective products was characterized by IR and elementary analysis.