Tuesday, 11 October 2011

1P19: q) Chemical and Enzymatic Synthesis of Fructose Analogues

 L. Azéma et al.51 synthesized various D-fructose analogues modified at C-1 or C-6 positions from D-glucose as probes for import studies by the hexose transporter in parasites e. g. Trypanosoma brucei by taking advantage of the Amadori rearrangement or using the aldol condensation between dihydroxyacetone phosphate and appropriate aldehyde catalyzed by fructose 1, 6-diphosphate aldolase from rabbit muscle. Rabbit muscle aldolase (EC 4.1.2.13) reversibly catalyzes the formation of fructose 1, 6-diphosphate from two triose-phosphates: dihydroxyacetone phosphate and D-glyceraldehyde 3-phosphate. This enzyme which is rather selective towards the dihydroxyacetone phosphate structure accepts a large variety of aldehydes as substrate and is frequently in use for synthetic purposes.52 Thus, the expected fructofuranosides (102-105) were chemoenzymatically synthesized starting from (R)-3-azido-2-hydroxypropanal diethyl acetal (101) (Scheme 19).53 Aldol condensation of 2-fold excess of aldehyde, resulting from deprotection of ketal (101), with dihydroxyacetone phosphate (formed in situ from fructose 1, 6-diphosphate) catalyzed by aldolase (1 mmol scale) gave the ketose-phosphate which was hydrolyzed in presence of acid phosphatase to yield 6-azido-6-deoxy-fructose (102) as unique reaction product. Subsequent ketalization of the azido ketose gave the corresponding methyl fructofuranoside (103) as a mixture of α- and β-forms. This compound allowed to obtain 6-amino-6-deoxy-fructose derivative (104), isolated after reductive amination, finally, sulfonylation of the ammonium salt with dansyl chloride,furnished the uorescent α- and β-methylfructofuranosides, 105a and 105b respectively. Attempts to obtain 105(a, b), through fructose derivative (107) starting from aldol condensation between dansyled (R) 3-amino-2-hydroxy-propanal diethylacetal 106 (obtained from 101) and dihydroxyacetone phosphate catalyzed by aldolase (Scheme 19) were unsuccessful. This is likely due to either the poor solubility of the aldehyde in aqueous solution or to the possible enzyme inactivation when high level of organic cosolvent was used to make the aldehyde soluble.



















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51. L. Azéma, F. Bringaud, C. Blonski, J. Périé, Bioorg. Med. Chem., 2000, 8, 717.
52. (a) C.-H. Wong, F. P. Mazenod, and G. M. Whitesides, J. Org. Chem., 1983, 48, 3493; (b) M. D. Bednarski, E. S. Simon, N. Bischofberger, W.-D. Fessner, M.-J. Kim, W. Lees, T. Saito, H.  aldmann, and G. M. Whitesides, J. Am. Chem. Soc., 1989, 111, 627; (c) J. M. Gijsen, L. Qiao, W. Fitz, and C.-H. Wong, Chem Rev., 1996, 96, 443.
53. a) P. Page, C. Blonski, and J. Périé, Tetrahedron, 1996, 52, 1557. b) T. Gefflaut, C. Blonski, J. Périé, and M. Willson, Prog.Biophys. Molec. Biol., 1995, 63,301; (c) J. Périé, I. Rivére-Alric, C. Blonski, T. Gefflaut, N. Lauth de Viguerie, M. Trinquier, M. Willson, F. R. Opperdoes, and M Callens, Pharmac. Ther., 1993, 60, 347; (d) T. Gefflaut, C. Blonski, and J. Périé, Bioorg. Med. Chem. 1996, 4, 2043; (e) C. Blonski, D. De Moissac, J. Périé, and J. Sygusch, Biochem. J.,1997, 323, 71.
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