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在氮气保护下,以多聚甲醛为原料,正丁醇作溶剂,三乙胺作助催化剂,在溴化-3-乙基苯并噻唑盐催化作用下合成了1,3-二羟基丙酮。考察了反应温度、反应时间、三乙胺用量对产物1,3-二羟基丙酮(DHA)收率的影响,得出的优选工艺参数为:60 mmol多聚甲醛,3 mmol催化剂和25 mL三乙胺,同时加入10 mL正丁醇,反应温度130℃,反应时间40 min。DHA收率为37%,选择性在95%～98%。产物经过先酯化再水解分离的提纯工艺,质量分数从90%提高到99.8%,分离提纯后得率为72%。产物熔点为73℃;通过IR、1HNMR及紫外可见光谱分析确证了化合物的结构。
1,3-Dihydroxyacetone was synthesized under the protection of nitrogen with paraformaldehyde as raw material, n-butanol as solvent and triethylamine as cocatalyst under the catalysis of 3-ethylbenzothiazolium bromide. The effects of reaction temperature, reaction time and amount of triethylamine on the yield of 1,3-dihydroxyacetone (DHA) were investigated. The optimum process parameters were as follows: 60 mmol paraformaldehyde, 3 mmol catalyst and 25 mL tris Ethylamine, while adding 10 mL n-butanol, the reaction temperature was 130 ℃, the reaction time was 40 min. DHA yield of 37%, selectivity of 95% to 98%. The product was esterified and then hydrolyzed to separate the purification process, the mass fraction increased from 90% to 99.8%, after isolation and purification yield was 72%. The melting point of the product was 73 ° C. The structure of the compound was confirmed by IR, 1HNMR and UV-Vis spectra.