- Stable isotope labeled methyltestosterone and synthetic method thereof
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The invention discloses stable isotope labeled methyltestosterone and a synthetic method thereof. The synthetic method comprises following steps: S1, stable isotope labeled methyl haloalkane is takenas a raw material and subjected to a reaction with magnesium powder in an organic solvent, and a stable isotope labeled Grignard reagent methyl magnesium halide is obtained; S2, 3-ethoxy-androsta-3,5-diene-17-one is taken as a raw material and subjected to an addition reaction with the Grignard reagent methyl magnesium halide prepared in S1 in the organic solvent, and a stable isotope labeled Grignard substance is generated; S3, the stable isotope labeled Grignard substance is subjected to acid-catalyzed hydrolysis in the organic solvent, and stable isotope labeled methyltestosterone is obtained. The steps of the synthetic method are simple, prepared stable isotope labeled methyltestosterone is easy to separate and purify, chemical purity can reach 99.0% or higher, isotope abundance is 98.0% atm or higher, and the national demand of quantitative detection for testosterone drugs is sufficiently met.
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Paragraph 0025; 0034; 0035; 0036; 0037; 0044; 0046
(2019/08/20)
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- Synthesis of deuterium labeled 17-methyl-testosterone
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The synthesis of two forms of selectively deuterated 17-methyl-testosterone is described. 17-Methyl-d3-testosterone was prepared by the Grignard reaction of dehydroepiandrosterone with deuterium labeled methyl magnesium iodide followed by an Oppenauer oxidation. 17-Methyl-d3-testosterone-19,19,19-d3 was prepared by treating 3,3-ethylenedioxy-5,10-epoxy-5α,10α-estran-17-one with deuterium labeled methyl magnesium bromide followed by hydrolysis and dehydration of the 5α-hydroxyandrostane derivative.
- Shinohara, Y.,Baba, S.,Kasuya, Y.
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p. 253 - 260
(2007/10/02)
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