Platinum (IV) oxide (Merck-Schuchardt,
Darmstadt) was reduced by hydrogen in glacial acetic acid. The reduced platinum
was used as a catalyst either after extensive washing with distilled water or
after evaporating the glacial acetic under a nitrogen stream. Ecdysone,
ecdysterone (both from Simes, Milano, Italy) or inokosterone (Rohto. Osaka,
Japan) were dissolved in distilled water (usually 1 mg/ml) and an equal amount
of reduced platinum was added. Oxygen was introduced into the solution through
a sintered glass disc and the mixture was continously stirred at room temperature.
The progress of oxidation was checked by thin-layer chromatography.
After thin-layer chromatography and scanning,
the radioactive peaks were scraped off and counted in a toluene cocktail
(Unisolve. Zinsser, Frankfurt) in a liquid scintillation counter (Betaszint,
Berthold and Frieseke, Karlsruhe). At the end
of oxidation the solutions were filtered, evaporated to dryness and dissolved
in methanol.
原料 蜕皮激素 和 氧化铂(IV)很好买到