- Synthesis of isotopically labeled fusarium mycotoxin 13C 2-moniliformin [1-hydroxycyclobut-1-ene-3,4-dione]
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The total synthesis of isotopically labeled [13C-1- hydroxycyclobut-1-ene-3,4-dione (moniliformin) a fungal toxic secondary metabolite to be used as internal standard for mycotoxin analysis is described. The synthesis proceeds in four steps starting from 1,4-dioxane, which was converted to 2,3-dihydro-1,4-dioxine followed by a [2+2]-cycloaddition with trichloroacetyl chloride-1,2-13Cas 13C source. The 13Clabeled cyclobutanone precursor was transformed to [ 13C-moniliformin by acid-catalyzed hydrolysis. The successful incorporation of two 13C atoms was proven by detailed NMR and mass spectrometric studies of labeled moniliformin and its precursor. Georg Thieme Verlag Stuttgart - New York.
- Lohrey, Lilia,Murata, Takeshi,Uemura, Daisuke,Humpf, Hans-Ulrich
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supporting information; experimental part
p. 2242 - 2244
(2011/10/31)
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- Syntheses, structure and conducting properties of halogenated ethylenedioxytetrathiafulvalenes
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4,5-Diiodo-, 4,5-dibromo-, and 4,5-dichloro-4′,5′-ethylenedioxytetrathiafulvalenes (EDO-TTFI2, EDO-TTFBr2, and EDO-TTFCl2) were synthesized in moderate to good yields by the two routes. The first route contains the reaction of EDO-TTF with LDA, followed by quenching with halogenated reagents, and the second route consists of the P(OR)3-mediated cross-coupling of 4,5-dihalogenated 1,3-dithiole-2-ones with 4,5-ethylenedioxy-1,3-dithiole-2-thione. The structures of EDO-TTFI2 and EDO-TTFCl2 were determined by X-Ray analysis. The radical-cation salts derived from EDO-TTFI2, EDO-TTFBr2, and EDO-TTFCl2 show high conductivities, although these compounds contain electron-withdrawing halogens as the substituent.
- Iyoda, Masahiko,Kuwatani, Yoshiyuki,Ogura, Eiji,Hara, Kenji,Suzuki, Hironori,Takano, Takahiro,Takeda, Koji,Takano, Jun-ichi,Ugawa, Kohei,Yoshida, Masato,Matsuyama, Haruo,Nishikawa, Hiroyuki,Ikemoto, Isao,Kato, Takehiro,Yoneyama, Naoki,Nishijo, Jun-ichi,Miyazaki, Akira,Enoki, Toshiaki
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p. 833 - 848
(2007/10/03)
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- DIISOPROPOXY- AND DI-tert-BUTOXYETHYNE STABLE ACETYLENE DIETHERS
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The rather stable acetylene diethers diisopropoxy- and di-t-butoxyethyne are prepared either from glyoxal or dioxane.Catalytic hydrogenation, acid-catalyzed hydration and formation of the corresponding hexacarbonyl dicobalt complexes are reported.
- Bou, Anna,Pericas,Miquel A.,Serratosa, Felix
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p. 1441 - 1449
(2007/10/02)
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