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有机化学
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有机化学 ›› 2010, Vol. 30 ›› Issue (9): 1391-1394. 上一篇    下一篇

研究简报

La(OTf)3催化合成1,3-二噁烷-4,6-二酮化合物的研究

严楠，熊斌，廖维林，许招会   

  1. (江西师范大学 江西省精细化工重点实验室 南昌 330027)
  • 收稿日期:2009-11-01 修回日期:2010-01-19 发布日期:2010-04-29
  • 通讯作者: 许招会 E-mail:gotoxzh@tom.com

Catalytic Synthesis of 1,3-Dioxane-4,6-dione by La(OTf)3

YAN Nan, XIONG Bin, LIAO Wei-Lin, XU Zhao-Hui   

  1. (Fine Chemical Key Laborary of Jiangxi Province, Jiangxi Normal University, Nanchang 330027)
  • Received:2009-11-01 Revised:2010-01-19 Published:2010-04-29
  • Contact: XU Zhao-Hui E-mail:gotoxzh@tom.com

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研究了在La(OTf)3的催化条件下, 以丙二酸和酮为原料, 缩合反应合成了3种1,3-二噁烷-4,6-二酮化合物. 考察了酸酮物质的量之比、反应温度、反应时间、催化剂用量及催化剂的稳定性等因素对反应的影响. 确定了其最佳反应条件为: 取0.1 mol丙二酸, n(丙二酸)∶n(酮)＝1.0∶1.1, 催化剂用量为0.3 mol%, 反应温度30 ℃, 反应时间为3.0 h, 在上述反应条件下, 产品收率可达62.3%～77.5%.

关键词: 1,3-二噁烷-4,6-二酮, 三氟甲基磺酸镧, 丙二酸, 酮

Three kinds of 1,3-dioxane-4,6-dione were synthesized from malonic acid and ketone using La(OTf)3 as catalyst and acetic anhydride as condensing regent. The effects of the molar ratio of malonic acid and ketone, reaction temperature, reaction time, catalyst dosage and its stability on the yield were investigated. The optimum conditions were as follows: 0.1 mol malonic acid, n(malonic acid)∶n(ketone)＝1.0∶1.1, the amount of catalyst 0.3 mol%, reaction temperature 30 ℃, reaction time 3.0 h. Under above reaction conditions, the product yields achieved up to 62.3%～77.5%.

Key words: 1,3-dioxane-4,6-dion, La(OTf)3, malonic acid, ketone