摘要
以对羟基苯甲酸、乌洛托品、多聚甲醛等为原料合成2-羟基-5-羧基间苯二甲醛,探讨了反应温度、时间、反应物用量及酸等因素对合成产率的影响。结果表明,较优反应条件为:在对羟基苯甲酸为0.02 mol的情况下,多聚甲醛用量为0.8 g、冰醋酸和乙酸酐用量分别为15 mL和8 mL,乌洛托品与对羟基苯甲酸的摩尔比为3,反应时间4.0 h、温度为120℃,此时反应产率可达78.9%,产品纯度达97.1%。产品经液-质联用仪和红外光谱仪表征无误。
2-Hydroxy-5-Caroxylisophthalaldehyde was synthesized by reaction of p-hydroxbenzoic acid,hexamethylenetetramine and paraformalclehyde.The optimum condition are as follows: n(urotropine)/n(p-hydroxbenzoic acid)=3:1,the reaction time being about4.0 h,temperature being about 120 ℃,the amount of the paraformalclehyde being 0.8 g,and glacial acetic acid 15 mL,and acetic anhydride 8mL.The yield can reach 72.8%.The product was characterized by LC-MS and IR.
出处
《化工生产与技术》
CAS
2011年第5期24-26,8,共3页
Chemical Production and Technology
