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    • 70. 发明授权
    • Purification of tetrahydrodibenzo[b,d]pyrans from crude synthetic
mixtures
    • 从粗制合成混合物中纯化四氢二苯并[b,d]吡喃
    • US4381399A
    • 1983-04-26
    • US332644
    • 1981-12-21
    • Robert E. OlsenStephen J. Backlund
    • Robert E. OlsenStephen J. Backlund
    • C07D311/00C07D20060101C07D311/80
    • C07D311/80
    • (-)-6a,10a-Trans-1-hydroxy-3-n-pentyl-6,6,9-trimethyl-6a,7,8,10a-tetrahydrodibenzo[b,d]pyran or any of its related pyrans in which the n-pentyl group is replaced by hydrogen or C.sub.1 -C.sub.10 alkyl is isolated from a crude synthetic mixture by a process which comprises esterifying the mixture to form perfluorinated alkanoic acid esters, removing low-boiling and non-volatile components, passing the mixture through a first gas chromatographic column with a packing whose liquid phase consists of a slightly polar phenyl-substituted silicone oil and recovering a fraction rich in the desired component, passing the recovered fraction through a second gas chromatographic column with a packing whose liquid phase consists of a non-phenyl-substituted silicone oil and recovering a fraction rich in the desired component, hydrolyzing the fraction recovered from the second stage, and recovering the desired product from the hydrolysis mixture.
    • ( - ) - 6a,10a-反式-1-羟基-3-正戊基-6,6,9-三甲基-6a,7,8,10a-四氢二苯并[b,d]吡喃或其相关的吡喃 其中正戊基被氢代替或C1-C10烷基通过包括将混合物酯化形成全氟化的链烷酸酯的方法从粗合成混合物中分离出来,除去低沸点和非挥发性组分,将 混合物通过具有填料的第一气相色谱柱,其液相由稍微极性的苯基取代的硅油组成并回收富含所需组分的级分,使回收的级分通过第二气相色谱柱,其中液相包含 的非苯基取代的硅油,并回收富含所需组分的级分,水解从第二级回收的级分,并从水解混合物中回收所需产物。