固载化卡宾催化剂合成1,3-二羟基丙酮

通过一种由二氧化硅或聚苯乙烯树脂固载化的卡宾催化剂催化甲醛缩合制备1,3-二羟基丙酮(DHA),在合成过程中不使用含有卤素的溴化3-乙基苯并噻唑盐和有毒有害的三乙胺,同时催化剂能够分离回收重复使用。在N2保护下,考察了反应温度、反应时间和不同溶剂对产物1,3-二羟基丙酮收率的影响。采用HLPC分析方法对DHA定量分析,在反应温度140℃,反应时间3 h和以二氧六环为溶剂的体系中,甲醛转化率可达100%,1,3-二羟基丙酮选择性为92.37%,并通过~1HNMR,~(13)CNMR及IR光谱分析确证了化合物的结构。

Synthesis of 1,3-dihydroxyacetone catalyzed by immobilized carbenecatalyst

1,3-Dihydroxyacetone(DHA) was prepared by condensation of formaldehyde over carbenecatalyst immobilized in silica or polystyrene resin.The synthesis process was free of 3-ethyl benzothiazole hydrochloric and triethylamine.The catalyst could be separated and recycled.Under the protection of nitrogen,the effects of reaction temperatures,reaction time and different solvents on DHA yield were investigated.The as-prepared DHA was quantitatively analyzed with HLPC analytical method.Under the condition of reaction temperature 140 ℃,reaction time 3 h and dioxane as solvent system,the conversion of formaldehyde reached 100%,and the selectivity to DHA was up to 92.37%.The structure of the compound were confirmed by ¹HNMR,¹³CNMR and IR spectroscopy.