bluuebunny/crossref_metadata_2025_split huggingface dataset:
The preparation and purification of 3–(4‐iodophenoxy)‐1‐isopropylamino‐2‐propanol‐125I, a beta adrenergic antagonist
Authors: Bobik A. , Woodcock E. A. , Johnston C. I. , Funder W. J. 
Published: October 2006

AbstractThe preparation of an iodine‐125 labelled beta adrenergic ligand, 3–(4‐iodophenoxy)‐1‐isopropylamino‐2‐propanol, suitable for β‐adrenergic receptor membrane binding studies is described. Several preparations have been carried out with radiochemical yields of 20–30%. Specific activities in the order of 150 Ci/mmol are readily obtained.
Synthesis of trideuterated testosterone labeled selectively at the C‐19 angular methyl group
Authors: Baba S. , Shinohara Y. , Kasuya Y. 
Published: October 2006

AbstractA synthetic procedure for testosterone‐19, 19, 19‐d3 is described. Deuterium labeling of the C‐19 position was achieved by the Grignard reaction of 17β‐acetoxy‐5α, 10α‐epoxy‐estrane‐3‐cycloethyleneketal with deuterium labeled methyl magnesium bromide (CD3MgBr). The synthesis resulted in a product with 97.8% d3 isotopic purity, which is selectively deuterated at C‐19 and chemically pure.
Preparation of [1‐14C]‐ and [9,10‐3H]‐Trans‐9‐Octadecenoic Acids from the Corresponding cis‐Compounds
Authors: Christie William W. 
Published: October 2006

Abstract[1‐14C]‐Trans‐9‐octadecenoic acid was obtained in 60 per cent overall yield and [9,10‐3H]‐trans‐9‐octadecenoic acid in 30 percent yield by stereomutation of the double bonds in the corresponding cis ‐compounds with nitrous acid in toluene. The products were purified by silver nitrate chromatography and contained no detectable positional isomers.
125I‐Labeled 1‐(2′‐acetyl‐4′‐[ortho‐iodobenzoyl]‐aminophenoxy)‐3‐isopropyl‐ aminopropan‐2‐ol
Authors: Hanson Robert N. , Davis Michael A. , Holman B. Leonard 
Published: October 2006

AbstractThe preparation of the iodine‐125 labeled beta adrenergic antagonist, 1‐ (2′‐acetyl‐4′‐[ortho‐iodobenzoyl] ‐aminophenoxy)‐3‐isopropylamino‐propan‐2‐ol, suitable for biodistribution studies is described. Synthesis of the unlabeled precursor proceeds in a 44% yield and the iodine‐125 exchange results in 89% incorporation of label. The final product is radiochemically pure (98‐99%) with a specific activity of 3.2 Ci/mmol.
11C‐Labelled radiopharmaceuticals: Synthesis and high pressure liquid chromatography of nicotinic‐11C acid amide
Authors: Machulla H.‐J. , Dutschka K. 
Published: October 2006

AbstractStarting with 11CO2, [carboxyl‐11C]‐nicotinic acid amide was synthesized via 3‐pyridyl‐lithium in practically carrier‐free amounts within 60 minutes. Overall radiochemical yields between 20% and 30% were obtained. Identification and purification of the labelled product was carried out by high pressure liquid chromatography using water as eluent.
Synthesis of carbon‐14 and carbon‐13 labeled chlorinated polycyclic pesticides
Authors: Heys J. R. , Duncan W. P. , Perry W. C. , Ebert D. A. , Radolovich G. , Haile C. L. 
Published: October 2006

AbstractThe preparations of the pesticides 1,1a,2,2,3,3a,4,5,5,5a,5b,6‐dodecachlorooctahydro‐1,3,4‐metheno‐1H‐cyclobuta[cd]pentalene‐U‐C14 (mirex‐U‐C14), 1,1a,3,3a,4,5,5,5a,5b,6‐decachlorooctahydro‐l,3,4‐metheno‐2H‐cyclobuta[cd]pentalen‐2‐one‐U‐C14 (Kepone™‐U‐C14), ethyl 5‐(1,1a,3,3a,4,5,5,5a,5b,6‐decachlorooctahydro‐2‐hydroxy‐l,3,4‐metheno‐1H‐cyclobuta[cd]pentalen‐2‐Y1‐1,1a,2,3,3a,4,5,5a,5b,6‐C1410)‐ levulinate (kelevan‐C14), 1,4,5,6,7,8,8‐heptachloro‐3a,4,7,7a‐tetra‐hydro‐4,7‐methanoindene‐4,5,6,7,8‐C514 (heptachlor‐4,5,6,7,8‐C514) and 1,4,5,6,7,8,8‐heptachloro‐2,3‐epoxy‐3a,4,7,7a‐tetrahydro‐4,7‐methanoindan‐4,5,6,7,8‐C514 (heptachlor epoxide‐4,5,6,7,8‐C514) from hexachlorocyclopentadiene‐U‐C14 are described. Specific activities were in the range of 1.8 to 3.2 mCi/mmol.Further, the synthesis of mirex‐C213 and Kepone™‐C213 from isopropyl formate‐C13 is reported. The determination of the carbon‐13 enrichment of these compounds was accomplished by selected ion monitoring (SIM) of seven ions in the molecular clusters of mirex and Kepone™, followed by calculation of the relative abundance of the various carbon‐13 containing molecules from the areas of the SIM plots.
The synthesis of non‐exchangeable deuterated internal standards for imipramine and its metabolites
Authors: Woodard R. W. , Craig J. Cymerman 
Published: October 2006

AbstractThe synthesis of 10,11‐dihydro‐5‐(3‐dimethylaminopropyl)‐5H‐dibenz[b,f]azepine (imipramine) and its 3‐methylamino analogue (desipramine)labelled with deuterium in either the 1‐ or the 3‐position of the side chain in high isotopic purity is described. The 3,3‐d2 compounds are obtained from the common precursor 5‐(2‐cyanoethyl)‐10,11‐dihydro‐5H‐dibenz[b,f]azepine by reduction and alkylation, while the 1,1‐d2 products are accessible from the 5‐(3‐chloropropionyl) derivative by amination and reduction. These compounds are required for use as non‐exchangeable mass spectrometric stable isotope internal standards for the simultaneous determination of imipramine and desipramine in biological fluids.
Synthesis of trans‐2,2‐Dimethyl‐3‐phenyl‐4‐(p‐β‐pyrrolidinoethoxy)phenyl‐7‐methoxy‐[2‐14C]chroman
Authors: Kole P. L. , Ray Suprabhat 
Published: October 2006

AbstractThe synthesis of trans‐2,2‐dimethyl‐3‐phenyl‐4‐(p‐β‐pyrrolidinoethoxy) phenyl‐7‐methoxy‐[2‐14C]chroman (Centchroman), a post‐coital antifertility agent from [1‐14C]phenylacetic acid is reported.
Synthesis of 2‐14c‐labelled 3H‐1,4‐benzodiazepines
Authors: Tegyey Z. S. , Maksay G. , Ötvös L. 
Published: October 2006

Abstract2‐14C‐oxazepam (7) 2‐14C‐(+)‐ and ‐(‐)‐7‐chloro‐1‐methyl‐5‐phenyl‐1,3,4,5‐tetrahydro‐3H‐1,4‐benzodiazepine‐2‐one (8a and 8b) as well as 2‐14‐7‐chloro‐4‐carbamoyl‐1‐methyl‐5‐phenyl‐1,3,4,5‐tetrahydro‐3H‐l,4‐benzodiazepine‐2‐one (9) were synthesised from carbobenzoxy‐glycine‐1‐14C. The overall radiochemical yields from carbobenzoxy‐glycine‐1‐14C were 28.9 % (7), 9.5 % (8a and 8b) and 25.3 % (9), respectively.
Convenient syntheses of N‐CD3 labelled nicotine and nicotine analogues
Authors: Seeman Jeffrey I. , Secor Henry V. , Forrest Gary 
Published: October 2006

AbstractTwo procedures for the preparation of N‐CD3 labelled nicotine and nicotine analogues are reported. These include: (a) the deuteroiodomethylation of the lithium amide of the corresponding secondary amine; and (b) the alkylation of the corresponding cyclic imine followed by sodium cyanoborohydride reduction of the resulting alkyl iminium salt. Products having both high chemical and isotopic purity are formed.
Synthesis of labelled histamine H2‐receptor antagonists I. Synthesis of deuterium, sulfur and tritium labelled cimetidine and metiamide by exchange
Authors: Hesselbo T. , Slade S. W. , Villani A. J. , Petka L. 
Published: October 2006

AbstractThe H2‐antagonists, metiamide and cimetidine were lahelled with deuterium and tritium in the 2‐position of the imidazole ring by the uncatalyzed exchange reaction with deuterium and tritium oxide at 100°C. The sulfur‐35 labelled metiamide was prepared by an exchange reaction with elemental sulfur‐35 in refluxing pyridine and by the reaction of 2[(4‐methyl‐5‐imidazolyl)methylthio]ethylamine with methylisothiocyanate‐35S in refluxing ethanol.
Labelled organophosphorus pesticides. III. Synthesis of carbon‐14 labelled o‐(2,6‐dichloro‐4‐methylphenyl) O,O‐dlmethyl phosphorothioate
Authors: Yoshitake Akira , Kanamaru Hiroshi , Shono Fumiaki , Nakatsuka Iwao 
Published: October 2006

AbstractO‐ (2,6‐Dichloro‐4‐methylphenyl) O,O‐dimethyl phosphorothioate (5‐3349) (1), a fungicide in soil, was labelled with carbon‐14 individually at the aryl methyl and the phenyl ring for use in metabolic studies. The synthetic procedures are illustrated in Fig. 1. 4‐Cyano‐14C‐phenol was quantitatively converted to 4‐methyl‐14C‐Phenol (3a) by catalytic hydrogenation using 10% Pd‐C as a catalyst. Dichlorination of 3a with chlorine gave 2,6‐di‐chloro‐4‐methyl‐14C‐phenol (4a). Condensation of 4a with O,O‐dimethyl phosphorochloridothioate gave S‐3349‐(aryl methyl‐14C) (1a) in the overall yield of 22% from potassium cyanide‐14C. By the similar procedures, 4‐methylphenol‐14C6 (3b) was converted to S‐3349‐(Phenyl‐14C6) (1b) in 70% yield.
The synthesis of cholesterol‐2,2,4,4,6‐d5
Authors: Gruenke Larry D. , Craig J. Cymerman 
Published: October 2006

AbstractCholesterol‐3,4‐d2 and ‐2,2,4,4,6‐d5 have been synthesized from Δ4 ‐ cholestene‐3‐one for use as mass spectrometric stable isotope internal standards. Conversion of Δ4 >‐cholesten‐3‐one to the enol acetate followed by reduction with sodium borodeuteride in a deuterated solvent yielded cholesterol‐3,4‐d2. Similarly Δ4‐cholesten‐3‐one‐2,2,4,6,6‐d5 obtained by base‐catalyzed exchange of Δ4‐cholesten‐3‐one in ethanol‐O‐d1 was converted to the enol acetate, followed by reduction with sodium borohydride in a deuterated medium to give cholesterol‐2,2,4,4,6‐d5.
Synthesis of the labeled gibberellin, GA9‐17‐14C
Authors: Lin Jiann‐Tsyh , Heftmann Erich 
Published: October 2006

AbstractGA9‐17‐14C was synthesized by introducing 14C into GA9‐17‐norketone by the Wittig reaction. The NMR and mass spectra of free GA9 and GA9‐17‐norketone are presented. The diphenylmethyl‐14C‐phosphine oxide is formed as a byproduct.
Rapid synthesis of 2‐deoxy‐D (1‐14C) glucose suitable for labelling with 11C
Authors: Mestelan Geneviève , Aubert Francis , Beaucourt Jean‐Pierre , Comar Dominique , Pichat Louis 
Published: October 2006

AbstractD‐arabitol (I) treated with acetone gave 2,3–4,5 and 1,2–4,5 di‐O‐isopropylidene‐D‐arabitol (II) as shown by 13C NMR. This mixture was converted into the corresponding mixture of mesylates from which 2,3–4,5‐di‐0‐isopropylidene‐1–0‐methane sulfonyl‐D‐arabitol (III) was isolated. The latter was converted into 1‐deoxy‐2,3–4,5‐di‐O‐isopropylidene‐1‐iodo‐D‐arabitol (IV). (IV) and sodium (14C) cyanide gave 2‐deoxy‐3,4–5,6‐di‐0‐isopropylidene‐D‐(1‐14C)‐glucononitrile (V) which was hemihydrogenated into 2‐deoxy‐D‐(1‐14C)‐glucose (VI). The overall yield based on sodium‐(14C)‐cyanide was 30 % and the radiochemical purity was 98 %. The overall time of synthesis was about one hour. This is suitable for working with 20 minutes halflived 11C.
Preparation of L‐cysteine‐35S hydrochloride by reduction of L‐cystine‐35s
Authors: Skakun‐Todorovi M. B. , Albahari S. R. 
Published: October 2006

AbstractThe method for the synthesis of L‐cysteine hydrochloride labelled with 35S is described. L‐cystine‐35S obtained from baker's yeast was reduced with tin in hydrochloric acid and radiochemically pure L‐cysteine‐35S hydrochloride was isolated by ion‐exchange chromatography on a column.The obtained L‐cysteine‐35S hydrochloride was stable in aqueous solution, pH 2, for six months and had specific activity of 20–125 mCi/mmol and radiochemical purity better than 95%.
Synthesis of glycyl‐L‐prolyl‐L‐leucyl‐[14C(U)] glycyl‐L‐proline as a substrate for collagenase
Authors: Lam‐Thanh Hung , Heindl Marie‐Christine , Fermandjian Serge 
Published: October 2006

AbstractThe synthesis of the 14C labelled peptide glycyl‐L‐leucyl‐[14C(U)] glycyl‐L‐proline (I) with the specific activity of 50 μCi/mMole was performed by the Merrifield solid phase method. The peptide (I) was degraded by Achromobacter iophagus collagenase.
Nouvelles Syntheses du Chloropractolol: Marquage au 14C, 2H, 3H
Authors: Pilichowski Jean‐François , Godeneche Denise 
Published: October 2006

AbstractLe chlorure de l'acide chloracétique(1‐14C a été obtenu, avec de bons rendements, par réaction d'échange entre le chlorure de benzoyle et l'acide chloracétique‐[1‐14C]. L'acylation de l'[(amino‐4 phénoxy)‐l, isopropylamino‐3, propanol‐2], par Ie réactif ainsi préparé a permis d'obtenir Ie Chloropractolol [1‐14C]avec une activité spécifique de 230 μCi/mmole. Nous décrivons également la synthèse du Chloropractolol deutérié et tritié (Activité Spécifique : 6,1 mCi/mmole) sur la position géminée avec le groupement hydroxyle.
The labeling of 4‐alkylamino‐iodoquinolines with radioactive iodine by isotopic exchange
Authors: Bakker Cees N. M. , Kaspersen Frans M. 
Published: October 2006

Abstract4‐alkylamino‐iodoquinolines can be labeled as their phosphate salts in high yields and in a short period of time by nucleophilic exchange in a melt with radioactive iodide. The iodide must be free of NaCl and reducing agents.
General methods for the synthesis of methyl isotope labelled catecholamine metabolites. Preparation of 4‐hydroxy‐3‐methoxy‐d3‐ (mandelic acid, phenylacetic acid, and phenylethylene glycol)
Authors: Markey S. P. , Powers K. , Dubinsky D. , Kopin I. J. 
Published: October 2006

AbstractTwo general schemes for the synthesis of isotope labelled monomethyl catecholamine metabolites are described. Catechol was converted to 2‐methoxy‐d3‐phenol (2) with deuteromethyl iodide and reacted with sodium glyoxylate to form 4‐hydroxy‐3‐methoxy‐d3‐mandelic acid (3). Hydrogenolysis of the methyl ester‐diacetate of 3 with excess sodium borohydride in water yielded 4‐hydroxy‐3‐methoxy‐d3‐phenylacetic acid (4). Reduction of 3 with diborane produced 4‐hydroxy‐3‐methoxy‐d3‐phenylethylene glycol (5). An alternative route was to alkylate 3,4‐dihydroxybenzaldehyde (6) and produce 3 or its 3‐hydroxy‐4‐methoxy isomer via the nitrile mandelic acid synthesis. Suitability of these isotopic and isomeric variants as internal standards for quantitation by gas chromatography‐mass spectrometry is discussed.
Synthesis of 5‐deuteromethyl‐2′‐deoxyuridine (thymidine‐α,α,α‐d3) and related compounds
Authors: Shiue C.‐Y. , Wolf A. P. , Slatkin D. N. 
Published: October 2006

AbstractThymine‐α,α,α‐d3 (4) was synthesized from perdeuterated methyl iodide and pyrimidine‐lithium. Thymidine‐α,α,α‐d3 (8) was then synthesized by coupling compound 4 with 1α‐chloro‐2‐deoxy‐3,5‐bis(p‐toluoyl)‐α‐D‐ribofuranosyl chloride in the presence of Friedal‐Crafts catalyst. Thymidine‐α,α,α‐d3 (8), a metabolic precursor of deoxyribonucleic acid, has potential application for study of human tissue growth kinetics in vivo using a sensitive deuterium micromapping technique.
Synthese De Phospholipides Marques Au Carbone 14 A l'aide Du “pyrophosphate D'Enediol Cyclique”
Authors: Danan J.‐L. , Pichat L. 
Published: October 2006

Abstract14C labelled phospholipid synthesis through the use of “cyclic enediolpyrophosphate”.Ramirez's phrophosphate 1 was used in a one pot convenient synthesis of a few [1‐14C]‐acyl phospholipids. Reagent 1 was condensed with 1,2‐[1‐14C] dipalmitoyl Sn‐glycerol to the cyclic triester phosphate 4 which without isolation, was reacted with N‐tritylethanolamine, 3‐0‐benzyl Sn‐glycerol and glycerol leading to intermediates 5, 6, 7 which were deprotected by triethylamine hydrolysis and other appropriate treatments.
A convenient synthesis of 13C‐bromoform and 13C‐tetrabromomethane from 13C‐iodomethane labelling through 13:CBr2
Authors: Siegel Herbert , Seebach Dieter 
Published: October 2006

AbstractPhenyldithiane 3 is methylated with 13CH3I to give, through the thioacetal 4, labelled acetophenone (5). NaOBr‐cleavage to the title compounds 1 and 2 (65 % and 76 %, respectively) and their use in the preparation of the dibromocyclopropane 6 and the dibromoolefin 7 are described.
Syntheses De γ, γ‐Dimethyl α‐Methylene‐γ‐ Butyrolactone Et d'oxa‐1 Spiro [4,5] Methylene‐3 Decanone‐2 Marquees Au Carbone‐14
Authors: Schlewer Gilbert , Stampf Jean‐Luc , Benezra Claude 
Published: October 2006

Abstract14C‐labelled γ, γ‐dimethyl‐α‐methylene‐γ‐butyrolactone 1 and 1‐oxa‐Spiro [4.5]‐3‐methylene‐2‐decanone 2 have been synthesized from acetone and cyclohexanone respectively and 14C‐labelled ethyl bromomethacrylate (Réformatsky reaction). The synthesis of this last compound is also described.
Preparation of 17β‐hydroxy‐[1ξ,2ξ‐3H2]4,6‐Androstadien‐3‐one
Authors: Taylor Clinton A. , Danzo Benjamin J. , Smith Howard E. 
Published: October 2006

Abstract17β‐Hydroxy‐[1ξ,2ξ‐3H2]4,6‐androstadien‐3‐one was prepared by the selective reduction of 17β‐hydroxy‐1,4,6‐androstatrien‐3‐one in benzene with tritium over 5% palladium on carbon. After purification by thin layer chromatography and high pressure liquid chromatography, the specific activity was at least 37 Ci/mmol, and the radiochemical purity was greater than 96%.
Reactions of metal carbonyl complexes. XII. Synthesis of 13C‐labelled (η6‐benzene)chromium(O) chalcocarbonyl complexes: (η6‐C6H6)Cr(13CO)3 and (η6‐C6H6)Cr(13CO)2(CX) (X = S, Se)
Authors: English Ann M. , Plowman Keith R. , Butler Ian S. 
Published: October 2006

Abstract13C‐Labelled (η6‐benzene)tricarbonylchromium(0), BzCr(13CO)3 (Bz = η6‐C6H6), has been prepared in about 50% yield with greater than 90 atom% 13C‐enrichment by a multistep, photochemically‐induced exchange of the three carbonyl groups in BzCr(CO)3 with 13CO. The syntheses of the closely related, 13CO‐labelled, thiocarbonyl and selenocarbonyl derivatives, BzCr(13CO)2(CX) (X = S, Se), from BzCr(13CO)3 are also described.
Marquage Par 14C Du[(Chloro‐2‐Ethyl)‐3 Nitroso‐3 Ureido]‐1′ Tri‐O‐Acetyl‐2′,3′,4′ α,β D‐Ribopyrannose Ou R.P.C.N.U.
Authors: Moreau M. F. , Madelmont J. C. , Godeneche D. 
Published: October 2006

AbstractRPCNU was labelled with 14C on three positions:

‐ On the carboxyl of the acetyl groups
‐ On the carboxyl of the acetyl groups
‐ On the urea carbonyl
Production of 13N‐labelled molecular nitrogen for pulmonary function studies
Authors: Vaalburg W. , Steenhoek A. , Paans A. M. J. , Peset R. , Reiffers S. , Woldring M. G. 
Published: October 2006

AbstractA method for the production of 13NN either as a gas or as an injectable solution is described. The method is based on the 16O(p,α)13N reaction and water as target material. Following irradiation, the 13NO and 13NO are reduced to 13NH3, followed by NaOBr oxidation to 13NN. With a beam current of 1 μA and 20 min irradiation time the injectable solution contained 148 MBq (4 mCi) per ml.
The preparation of tritium and deuterium‐labelled camptothecin
Authors: Ronman Peter E. , Wani Mansukh C. , Wall Monroe E. 
Published: October 2006

AbstractThe synthesis of d, l, ‐12‐bromocamptothecin (2d) from camptothecin (1) is described. Reduction of the bromo derivative 2d with tritium gas in the presence of palladium on carbon afforded d, l‐camptothecin 12‐3H having a specific activity of 29 Ci/mmol. A simpler labelling procedure was subsequently discovered whereby deuterium in the presence of palladium on carbon reduced ring B of camptothecin and also exchanged the C‐5 hydrogen with deuterium. The reduced camptothecin aromatized to camptothecin in the presence of air to give deuterium incorporation in the C‐5 and C‐7 positions.
A versatile procedure for the preparation of palmitic acid‐d2 and stearic acid‐d6
Authors: Adlof R. O. , Emken E. A. 
Published: October 2006

AbstractSyntheses of palmitic acid‐d2 and stearic acid‐d6 are described, the latter route also having the capability of producing methyl oleate and elaidate‐13,13,14,14‐d4 from the same synthetic sequence. Overall yields are in the range of 40 to 60%. These syntheses use tris (triphenylphosphine) ‐ chlororhodium(I) for the incorporation of deuterium. Atomic absorption spectroscopy is used to confirm that less than 70 ppb rhodium catalyst remained in the final products.
Synthesis of 14C and 3H specifically labelled 1‐benzyl‐4‐ ‐picolinoyl‐piperazine
Authors: Zólyomi G. , Budai Z. 
Published: October 2006

AbstractSpecifically labelled 1‐benzyl‐4‐picolinoyl‐piperazine (4) was synthetized for use in metabolism studies. Carbon‐14 was introduced both in benzyl and picolinoyl groups, and tritium in the benzyl group. By using commercial n‐butyllithium in n‐hexane, the yield of picolinic acid was improved.
A rapid and convenient method for specific 11C‐labelling of synthetic polypeptides containing methionine
Authors: Långström B. , Sjöberg S. , Ragnarsson U. 
Published: October 2006

Abstract11C‐labelling of methionine residues in a synthetic peptide via the preparation of the corresponding protected, pure homocysteine peptide has been investigated. Complete deprotection of the peptide and specific methylation of the homocysteine residue can be performed in one step in liquid ammonia. As a first application of this method the synthesis of the tripeptide, Z‐Gly‐L‐Hcy (Bzl)‐Gly‐O‐Bzl, and its conversion to Gly‐Met‐Gly and the corresponding labelled Gly‐([11C]‐methyl) ‐ Met‐Gly, is reported. Starting with the protected peptide the labelling was performed in 20 ± 5 min (starting with 11CO2), yielding the labelled peptide in 92 ± 5 % radiochemical yield. Analyses and preparative LC can be performed within 6 min.
The preparation of aromatic astatine compounds through aromatic mercury compounds part II: Astatination of pyrimidines and steroids
Authors: Visser Gerard W. M. , Diemer Eduard L. , Kaspersen Frans M. 
Published: October 2006

AbstractSeveral 211At‐astatopyrimidines (5‐At‐uracil, 5‐At‐cytosine and their nucleosides and nucleotides including DNA and RNA) have been synthesized in high radiochemical yields by reaction of 211At/I2 and the corresponding chloromercury compounds. Also some astato‐steroids (6‐At‐cholesterol and 2‐ and 4‐astatoestradiol) have been prepared by this method. The stability in vitro was determined under different conditions in comparison with the analogous iodo compounds.
3‐[11C]‐methyl‐D‐glucose, a potential agent for regional cerebral glucose utilization studies: Synthesis, chromatography and tissue distribution in mice
Authors: Kloster G. , Müller‐Platz C. , Laufer P. 
Published: October 2006

Abstract3‐[11C]‐Methyl‐D‐glucose was synthetized by methylation via 11CH3I of the potassium salt of diacetone‐D‐glucose; hydrolysis of the ketal groups with HCl yields 3‐[11C]‐methyl‐D‐glucose. The radiochemical yield is 35% at a specific activity of 1.9 mCi/μmole. Synthesis time including purification by hplc is about 30 min. Up to 12.0 mCi have been obtained in injectable solution.The tissue distribution of 3‐[11C]‐methyl‐D‐glucose was determined in mice at different times after an i.v. injection. All well‐perfused organs like lung, heart, liver, kidney and brain rapidly accumulate 3‐[11C]‐methyl‐D‐glucose. The accumulation in brain is significant: at 15 min after application it reaches 6.2% dose/g organ.
Synthesis of 1,5,9‐cyclododecatriene‐x‐14C6
Authors: Susán Alexander B. , Duncan William P. 
Published: October 2006

AbstractA small‐scale synthesis of 1,5,9‐cyclododecatriene‐x‐14C6 is described. 1,3‐Butadiene‐1,4‐14C2, specific activity of 1.15 mCi/mmole, was prepared via the thermal decomposition of tetramethylene‐1,4‐14C2‐bis‐(trimethylammonium hydroxide) and immediately converted to a mixture of stereoisomers of 1,5,9‐cyclododecatriene‐x‐14C6 using a Ziegler catalyst prepared in situ. The overall radiochemical yield was 15% (based on K14CN).
3H‐labelled bilirubin and biliverdin
Authors: Hutchinson David W. , Wilkes Nicola M. , Au Hilary Y. N. 
Published: October 2006

AbstractA simple method is described for the preparation of [3H]bilirubin IX‐α by the reduction of biliverdin IX‐α using sodium boro[3H]hydride. The [3H]bilirubin is obtained with a high specific radioactivity and the tritium is located at the methylene bridge (C‐10). Oxidation of the [3H]bilirubin with chloranil results in some loss of tritium from C‐10 and [3H]biliverdin is obtained.
Tritium labeled prostacyclin sodium salt
Authors: Hsi Richard S. P. , Stolle Wayne T. , McGrath James P. , Morton Douglas R. 
Published: October 2006

AbstractCrystalline [11β‐3H]prostacyclin (PGI2) sodium salt (5) was prepared from prostaglandin D2 (PGD2) methyl ester (1). Reduction of PGD2 methyl ester with sodium borotritide afforded [11β‐3H]prostaglandin F2α (PGF2α) methyl ester (2a) in 57% radiochemical yield. [11β‐3H]PGF2α methyl ester was converted via (5R, 6R)‐ and (5S, 6S)‐5‐iodo‐[11β‐3H]prostaglandin I1 methyl ester (3) to [11β‐3H]‐prostacyclin methyl ester (4). Carefully controlled hydrolysis of 4 produced crystalline [11β‐3H]PGI2 sodium salt which was shown to be >95% pure by means of high performance liquid chromatographic (HPLC) analysis. The overall yield from [11β‐3H]PGF2α methyl ester to [11β‐3H]PGI2 sodium salt was 53%. [11β‐3H]PGI2 sodium salt with a specific activity of 502 μCi/mg has only limited radiochemical stability. Its radiochemical purity declined 15% after three weeks of storage at −20°C in the crystalline state.