α-蒎烯合成2-羟基-3-蒎酮的研究
Study on Synthesis of 2-Hydroxy-3-Pinanone from α-Pinene
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摘要: 研究了高锰酸钾氧化α-蒎烯合成2-羟基-3-蒎酮的工艺条件,对助溶剂等影响因素进行了探讨,较优工艺条件为:以叔丁醇为助溶剂,不改变pH值,温度0~5℃,KMnO4与α-蒎烯的物质的量比为1.7:1~1.8:1,先加α-蒎烯后加KMnO4。所得2-羟基-3-蒎酮采用IR、MS、1H NMR、13CNMR 进行了表征,产率达 60%,与文献相同,助溶剂改用叔丁醇后回收率>90%,高于原用助溶剂丙酮(回收率 70%)。Abstract: The synthetic technology of 2-hydroxy-3-pinanone from α-pinene was studied. Affecting factors such as cosolvent were investigated. The optimum technology was obtained as follows:using tert-butyl alcohol as cosolvent, taking no measure to change pH value, reaction temperature 0-5℃, ratio of n(KMnO4):n(α-pinene) 1.7:1-1.8:1, addition of potassium permanganate after α-pinene. The structure of the product was characterized by IR, MS, 1HNMR and 13CNMR. The yield of 2-hydroxy-3-pinanone was up to 60%, ashigh as the literatures reported before. The recovery of tert-butyl alcohol washigher than 90%, which washigher than that of acetone (70%), the cosolvent used ever before.