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Hoehr, Cornelia ; Paulßen, Elisabeth ; Benard, Francois ; Lee, Chris Jaeil ; Hou, Xinchi ; Badesso, Brian ; Ferguson, Simon ; Miao, Qing ; Yang, Hua ; Buckley, Ken ; Hanemaayer, Victoire ; Zeisler, Stefan ; Ruth, Thomas J. ; Celler, Anna ; Schaffer, Paul
Access to promising radiometals as isotopes for novel molecular imaging agents requires that they are routinely available and inexpensive to obtain. Proximity to a cyclotron center outfitted with solid target hardware, or to an isotope generator for the metal of interest is necessary, both of which can introduce significant hurdles in development of less common isotopes. Herein, we describe the production of ⁴⁴Sc (t₁⸝₂ = 3.97 h, Eavg,β⁺ = 1.47 MeV, branching ratio = 94.27%) in a solution target and an automated loading system which allows a quick turn-around between different radiometallic isotopes and therefore greatly improves their availability for tracer development. Experimental yields are compared to theoretical calculations.
Werner, Frederik ; Groebel, Simone ; Wagner, Torsten ; Yoshinobu, Tatsuo ; Selmer, Thorsten ; Baumann, Marcus ; Schöning, Michael Josef
Es wird die Synthese der Sequenz A 6–9 des Schafinsulins in der geschützten Form Boc-Cys-Cys-Ala-Gly-OBuᵗ (5) sowie das Verhalten dieses monomeren cyclischen Cystinpeptidderivates gegenüber den in der Peptidchemie gebräuchlichen Reagenzien Bortrifluorid/Eisessig, Triäthylamin und Hydrazinhydrat beschrieben.
Zur Synthese der Hühnerinsulin-A-Kette, I : Darstellung der Fragmente A1–8, A9–15, A1–7 und A8–15
(1979)
Die tert.-Butyloxycarbonyl-Gruppe (Boc) läßt sich mittels reiner Trifluoressigsäure nicht selektiv neben dem Benzyloxycarbonyl-Rest (Z) abspalten. Das gelingt auch nicht mit Lösungen von Trifluoressigsäure bzw. Chlorwasserstoff in organischen Lösungsmitteln. Kern-substituierte Z-Gruppen wie Z(pCl), Z(mCl) oder Z(pNO₂) sind zwar stabiler, werden aber von den obengenannten Reagenzien ebenfalls angegriffen bzw. sind nicht mehr acidolytisch abspaltbar. – Mit 70proz. wäßriger Trifluoressigsäure gelingt die Abspaltung von Boc neben Z dagegen fast selektiv; dabei werden aber Benzylester, besonders Glutaminsäure-γ-benzylester, teilweise hydrolysiert, während Methyl- sowie Äthylester nahezu beständig sind. Die Brauchbarkeit des Abspaltungsverfahrens wird anhand der schrittweise durchgeführten Synthese zweier Heptapeptid-Derivate gezeigt. – Ähnlich spezifisch gelingt die Abspaltung von Boc mit Bortrifluorid-ätherat in Eisessig; Benzylester sind gegenüber diesem Reagenz stabiler als gegen wäßrige Trifluoressigsäure. Das Bortrifluorid-Verfahren eignet sich besonders für die Abspaltung von Boc-Gruppen neben säurelabilen Thiol-Schutzgruppen (Tetrahydropyranyl- bzw. Trityl-Rest) sowie neben dem Cyclocystinyl-Rest. Die Leistungsfähigkeit der Methode wird durch die Synthese zweier Peptid-Derivate mit S-Trityl-Schutzgruppen belegt. Als Nebenreaktion ist die Acetylierung von aliphatischen Hydroxylgruppen möglich. Sie läßt sich vermeiden, wenn man die Spaltung in anderen Lösungsmitteln durchführt. Die als Modellverbindungen für Stabilitätsuntersuchungen verwendeten Nε-acylierten Lysin-Derivate werden mit dem Aminosäureanalysator quantitativ neben Lysin bestimmt.