Purification of tetrahydrodibenzo[b,d]pyrans from crude syntheti

Details Purification of tetrahydrodibenzo[b,d]pyrans from crude syntheti Purification of tetrahydrodibenzo[b,d]pyrans from crude syntheti

1981-12-21

1983-04-26

Chan, Nicky

Organic compounds -- part of the class 532-570 series

Organic compounds

Heterocyclic carbon compounds containing a hetero ring...

210635, 210659, C07D31180

Patent

active

043813992

ABSTRACT:
(-)-6a,10a-Trans-1-hydroxy-3-n-pentyl-6,6,9-trimethyl-6a,7,8,10a-tetrahydro dibenzo[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.

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