摘要
以芳香醛(2a~2h)和亚膦酸二乙酯(3)为原料、三乙烯二胺(DABCO)为有机碱,采用研磨法一步合成α-羟基膦酸酯(1a~1h),通过^(1)HNMR对其结构进行了表征,并对合成条件进行了优化。结果表明,以目标化合物(苯基)(羟甲基)膦酸二乙酯(1a)的合成为模型反应,确定最佳合成条件如下:物料比n(亚膦酸二乙酯)∶n(苯甲醛)为1.8∶1、DABCO用量n(DABCO)∶n(苯甲醛)为0.5∶1、研磨时间为15 min,在此条件下,目标化合物1a收率达到83.6%。
Taking aromatic aldehydes(2a-2h)and diethyl phosphite(3)as raw materials,and triethylenediamine(DABCO)as an organic base,we synthesizedα-hydroxyphosphonate(1a-1h)by a one-step grinding method.Moreover,we characterized the structures of the target compounds 1a-1h by ^(1)HNMR,and optimized the synthesis conditions.The results show that while taking the synthesis of the target compound(phenyl)(hydroxymethyl)phosphonate diethyl ester(1a)as a model reaction,the yield of target compound 1a can reach 83.6%under the optimal synthesis conditions as follows:the material ratio n(diethyl phosphite)∶n(benzaldehyde)is 1.8∶1,the DABCO dosage n(DABCO)∶n(benzaldehyde)is 0.5∶1,and the grinding time is 15 min.
作者
赵梅梅
杜漠
高艳蓉
仝红娟
ZHAO Meimei;DU Mo;GAO Yanrong;TONG Hongjuan(Shaanxi Institute of International Trade&Commerce,Xi′an 712046,China;Collaborative Innovation Center of Green Manufacturing Technology for Traditional Chinese Medicine in Shaanxi Province,Xi′an 712046,China)
出处
《化学与生物工程》
CAS
2023年第7期27-29,33,共4页
Chemistry & Bioengineering
基金
陕西省教育厅2022年度专项科学研究计划项目(22JK0280)
陕西国际商贸学院校级项目(SMXY202123)。
