bluuebunny/crossref_metadata_2025_split huggingface dataset:
Synthesis of tritium labelled (−)‐3‐PPP, a selective dopamine autoreceptor agonist
Authors: Thorberg Seth‐Olov , Johansson Lars , Gawell Lars , Sahlberg Christer 
Published: October 2006

Abstract3H‐(‐)‐3‐PPP (11, (S)‐3‐(3‐Hydroxyphenyl)‐N‐propyl‐[3,4‐3H]piperidine) was prepared by hydrogenation of compound 3, with tritium gas followed by resolution of the racemic mixture. The incorporation of tritium was verified by tritium NMR spectroscopy. Also described is the synthesis and NMR interpretation of two isomeric unsaturated tetrahydropyridine derivatives i.e. compounds 8 and 10.
Labeled bile acids VI: [22,23,24‐13C3]‐methyl 3α,7α‐diacetoxy 5β‐cholan‐24‐oate, [22,23,24‐13c3]‐methyl 3β‐acetoxychol‐5‐en‐24‐oate, and [16,17,22,23‐3h4]‐methyl 3β‐acetoxychol‐5‐en‐24‐oate (1)
Authors: Lai Chee Kong , Byon Chang Yon , Anderson Warren G. , Gut Marcel 
Published: October 2006

AbstractA general short procedure for the introduction of 13C to the side chain of bile acids is described. Suitable (Z)‐pregn‐17(20)‐enes are key intermediates, while the isotope is introduced by an ene reaction with [1,2,3‐13C3]‐methyl propiolate. For the labeling with tritium, the unlabeled product of the ene synthesis, a Δ5,16,22‐triene was saturated selectively at 16,17 and 22,23 with tritium gas.
14C‐Labelling of prallethrin SF, (4S)‐1‐OXO‐2‐propargyl‐3‐methylcyclopent‐2‐en‐4‐yl (1R)‐CIS‐ and (1R)‐trans‐chrysanthemates
Authors: Kanamaru Hiroshi , Kawahara Kazuo , Kamada Takeshi , Yoshitake Akira , Nakatsuka Iwao 
Published: October 2006

AbstractBoth of the components of prallethrin SF [(4S)‐1‐oxo‐2‐propargyl‐3‐methylcyclopent‐2‐en‐4‐yl (1R)‐cis,trans‐chrysanthemate], a novel potent insecticidal pyrethroid, were labelled with carbon‐14 at the cyclopentenyl‐2 position for use in metabolic studies. Carbonation of 2‐lithio‐5‐methylfuran (4) with carbon‐14 dioxide (3) gave 5‐methyl‐2‐[carboxyl‐14C]furoic acid (5). Reduction of 5 with lithium aluminium hydride followed by oxidation with manganese dioxide afforded 5‐methyl[carbonyl‐14C]‐furfural (7). Modified Grignard reaction of 7 with propargyl bromide and magnesium in the presence of mercuric chloride yielded 1‐(5‐methyl‐2‐furyl)[1‐14C]but‐3‐yn‐1‐ol (8). Molecular rearrangement of 8 followed by isomerization afforded 2‐propargyl‐3‐methyl[2‐14C]cyclopent‐2‐en‐4‐ol‐1‐one (9) in 30% yield from barium [14C]carbonate (2). Direct optical‐resolution of 9 by preparative HPLC with a chiral‐phase column gave (+)‐(4S) and (‐)‐(4R) isomers (10 and 11) quantitatively. Condensation of 10 with (1R)‐cis‐ or (1R)‐trans‐chrysanthemoyl chloride (12a or 12b) yielded (4S),(1R)‐cis‐ or (4S),(1R)‐trans‐[cyclopentenyl‐2‐14C]prallethrin (1a or 1b). Both overall radiochemical yields of 1a and 1b were about 9% from 2.
A nine‐step synthesis of [14C]flupirtine maleate labeled in the pyridine ring
Authors: Choi Yong M. , Kucharczyk Norbert , Sofia R. Duane 
Published: October 2006

AbstractA nine‐step procedure for microscale synthesis of ethyl 2‐amino‐6‐{[(4‐fluorophenyl)methyl]amino}‐3‐pyridinyl‐2,6‐14C carbamate maleate [10], [14C]flupirtine maleate, was developed. The synthesis started with the readily avaiable and economical reagents, potassium cyanide‐14C and 1,3‐dibromopropane making the following intermediates: glutaronitrile‐14C [2], glutarimide‐14C [3], 2,6‐dichloropyridine‐2,6‐14C [4], 2,6‐dichloro‐3‐nitro‐pyridine‐2,6‐14C [5], 2‐amino‐3‐nitro‐6‐chloropyridine‐2,6‐14C [6], 2‐amino‐3‐nitro‐6‐(p‐fluorobenzylamino)pyridine‐2,6‐14C [7], 2,3‐diamino‐6‐(p‐fluoro‐benzylamino)pyridine‐2,6‐14C [8], and ethyl 2‐amino‐6‐{[4‐fluoropheny(l)‐methyl]amino}‐3‐pyridinyl‐2,6‐14C carbamic acid ester hydrochloride [9]. The overall yield was 6.3% (5.4 mCi), and the radioactivity was 99.8% as determined by high performance liquid chromatogrphy and liquid scintillation counting.
Preparation of carbon‐14, tritium and deuterium labelled terodiline, and carbon‐14 and deuterium labelled emepronium bromide
Authors: Werner Tom F. , Olsson Lars‐Inge 
Published: October 2006

AbstractSelectively ring‐labelled terodilines (N‐tert‐butyl‐1‐methyl‐3,3‐diphenylpropylamine; 1) were prepared by homogeneous catalytic exchange of aromatic hydrogens for 3H and 2H. In addition, terodilines specifically labelled with 14C, 3H or 2H were prepared from the appropriate 1‐methyl labelled 4,4‐diphenylbutan‐2‐ol, by treating the corresponding tosylates with tert‐butylamine.Emepronium bromide (N‐ethyl‐N,N,1‐trimethyl‐3,3‐diphenylpropylammonium bromide; 2) specifically labelled with 14C or 2H were similarly prepared by treating the labelled tosylates with N‐ethylmethylamine or dimethylamine, followed by quaternization with methyl bromide or ethyl bromide, respectively.
An improved synthesis of 14C labelled glycerol using sodium borohydride
Authors: Chander Harish , Ramamurthy T. T. , Viswanathan K. K. 
Published: October 2006

Abstract[1‐14C]Glyceric acid has been reduced to [13]‐14Clglycerol in high yields via the methyl ester of 1‐14Clglyceric acid by sodium borohydride in the presence of t‐butyl alcohol and methanol. The importance of the procedure is highlighted in relation to other procedures involving lithium aluminium hydride reduction.
Syntheses of no‐carrier‐added (NCA) [18F]fluoroalkyl halides and their application in the syntheses of [18F]fluoroalkyl derivatives of neurotransmitter receptor active compounds
Authors: Shiue C.‐Y. , Bai L.‐Q. , Teng R.‐R. , Wolf A. P. 
Published: October 2006

AbstractNucleophilic aliphatic substitution of alkyl halides, 1, [(CH2)nX2 (n=2, 3; X=Br,I)], with NCA K[18F]/Kryptofix 2.2.2 in CH3CN gave the corresponding NCA [18F]fluoroalkyl halides 2 in 30–40% yields. The factors which influence the yield of 2 were compared. N‐Alkylation of several neurotransmitter receptor active amides and amines with this reagent gave the corresponding NCA N‐[18F]fluoroalkyl derivatives (3–6) in 20–60% yield.
Synthesis of racemic [3‐11C]‐labelled alanine, 2‐aminobutyric acid, norvaline, norleucine, leucine and phenylalanine and preparation of L‐[3‐11C]alanine and L‐[3‐11C]phenylalanine
Authors: Antoni Gunnar , Långström Bengt 
Published: October 2006

AbstractThe syntheses of racemic [3‐11C]‐labelled alanine, 2‐amino‐butyric acid, norvaline, norleucine, leucine and phenyl‐alanine are reported. The reaction were performed by a phase‐transfer alkylation reaction on N‐(diphenylmethylene)‐glycine tert‐butyl ester with the appropriate 11C‐alkyl iodides followed by acidic hydrolysis and the labelled amino acids were obtained in 10‐55 % radiochemical yield. L‐[3‐11C]‐Alanine and L‐[3‐11C]phenylalanine were obtained in 99 % enantiomeric excess after treatment of the corresponding racemic mixture by D‐amino acid oxidase immobilized on glutaral‐dehyde‐activated glass beads.In a typical run starting with 120 mCi [11C]carbon dioxide, 25 mCi [1‐11C]benzyl iodide was prepared and used to give 6 mCi of DL‐[3‐11C]phenylalanine within 50 minutes. Following treatment with D‐amino acid oxidase, 0.3 mCi of L‐[3‐11C]phenylalanine was obtained after a total synthesis time of about 100 minutes.
Nuclear overhauser effects in tritium nmr
Authors: Kaspersen Frans M. , Funke Carel W. , Sperling Eric M. G. , Wagenaars Gerard N. 
Published: October 2006

AbstractThe accuracy of the quantification of the tritium distribution in labelled compounds may be reduced by differential nuclear Overhauser effects, especially for compounds in which the different tritiated positions differ in the number of protons surrounding them.
Synthesis of 1‐C2H3 theophylline and 3‐C2H3 theophylline
Authors: Berlioz C. , Falconnet J. J. , Desage M. , Brazier J. J. 
Published: October 2006

AbstractThis article describes a three step‐selective deuteration method of 1‐methyl and 3‐methylxanthine, after protection of the N‐7 position by chloromethylpivalate and alkylation by trideuteromethyl iodide; yielding 1‐C2H3 and 3‐C2H3 theophylline.
Synthesis of 2H8‐leukotriene B4
Authors: Dawson Michael , Vine John H. , Forrest Michael J. , McGee Colette M. , Brooks Peter M. , Watson Thomas R. 
Published: October 2006

AbstractA semi‐synthetic method for the preparation of deuterated leukotriene B4 (2H8‐LTB4) from eicosatetraynoic acid (ETYA) is described which involves reduction of ETYA to deuterated arachidonic acid (2H8‐AA) with deuterium gas and then biological conversion of this material to 2H8‐LTB4 by rat peritoneal polymorphonuclear leukocytes (PMNs).
Synthesis of 1‐(2‐ethoxyethyl)‐2‐(4‐methyl‐1‐homopiperazinyl)‐[2‐14C]benzimidazole difumarate([14C]KB‐2413)
Authors: Awata Norio , Satomi Osamu 
Published: October 2006

Abstract1‐(2‐Ethoxyethyl)‐2‐(4‐methyl‐1‐homopiperazinyl)‐[2‐14C]‐benzimidazole difumarate ([14C]KB‐2413), a new antihistaminic agent, was prepared from labelled urea.The synthetic intermediate, 1‐(2‐Ethoxyethyl)benzimidazolone, obtained in good yield by the condensation of N‐(2‐ethoxyethyl)‐o‐pheynylenediamine with [14C]urea, was chlorinated with phosphorus oxychloride and followed by the reaction with N‐methylhomopiperazine to give the base of [14C]KB‐2413. It was then converted to the difumarate, which was obtained in an overall radiochemical yield of 74% starting from [14C] urea.The specific activity was 54.4 mCi/mmol and its radiochemical purity was 98.0% in reverse isotope dilution analysis.
Preparation of [Thienyl‐3‐14C]temocillin
Authors: Freer R. , Hatt B. B. , Mitchell M. M. , Morecombe D. D. 
Published: October 2006

Abstract[thienyl‐3‐14C]Temocillin has been prepared from [1‐14C]chloroacetic acid via 3‐[3‐14C]thienylmalonic acid.
Synthesis of (5,6)‐epoxy‐(1α, 2β, 3α, 4β)‐(±)‐5‐cyclohexane‐ 1‐3H, 2,3, 4‐3H ‐tetrol. (3H ‐Conduritol B epoxide)
Authors: Gal Andrew E. , Voorstad Josée P. 
Published: October 2006

AbstractTritium labeled Conduritol B epoxide was prepared by a six step synthesis, starting with p‐benzoquinone. The tritium was introduced into the molecule in the second step by reducing the quinone with sodium boro 3H hydride.
Synthesis of deuterium labelled triazolobenzodiazepines
Authors: Koves G. J. 
Published: October 2006

AbstractAlprazolam and Triazolam ‐ anxyolitic and hypnotic agents ‐ were labelled with deuterium. First synthesis: through CD3COOD acylation of the appropriate Hydrazones, followed by thermal cyclization. Second synthesis: deuterium exchange through acid catalized carbocation intermediates in a CD3COOD/D2SO4 mixture. The products were used as internal standards for GC/MS/SIM quantitative analysis in forensic case work.
6‐Bis‐(2‐chloroethyl)amino‐6‐deoxy‐D‐[14C(U)]‐glucose
Authors: Thomas H. Jeanette , Montgomery John A. 
Published: October 2006

Abstract14C‐Labeled 6‐bis‐(2‐chloroethyl)amino‐6‐deoxy‐D‐glucose hydrochloride was prepared from D‐[14C(U)]‐glucose for DNA binding studies.
Preparation of [3H]N, N‐dimethylaniline by microwave discharge activation of tritium gas. Absence of ring saturation
Authors: Peng C. T. , Ding S. F. , Hua R. R. 
Published: October 2006

Abstract[3H]N, N‐Dimethylaniline was prepared from N, N‐dimethylaniline by tritium labeling by microwave discharge activation of tritium gas; the product was formed without any ring saturated side products. High specific activity and high yield were achieved by input of high microwave power to excite the plasma and by dispersion of substrate on silica‐alumina pellets to increase the contact surface with tritium gas. Circulation or no circulation of tritium gas during labeling did not effect the yield or the specific activity. Dispersion on supported Ni caused an increase in the specific activity of [3H],N, N‐dimethylaniline than on plain silica‐alumina. The lack of ring saturation in N, N‐dimethylaniline in contrast to complete ring saturation in N, N‐dimethylaniline in contrast to complete ring saturation in benzene and benzoic acid has been interpretated to indicate the involvement of tritium ions in addition to tritium atoms in tritium labeling.
Synthesis of cis‐diamino‐[1,1‐[1‐14C]cyclobutanedicarbonyloxy (2)‐0,0] platinum II
Authors: Haynes U. U. , Swigor J. J. , Pittman K. K. 
Published: October 2006

AbstractThe synthesis of the title compound (4) is described. [2‐14C]Diethyl malonate was treated simultaneously with a freshly prepared solution of sodium ethoxide and 1,3‐dibromopropane to give 1 1‐[1‐14C]cyclobutanedicarboxylic acid diethyl ester (1). Treatment with potassium hydroxide saponified the ester leaving the dipotassium salt (2). Conversion of potassium tetrachloroplatinate II with potassium iodide followed by ammonium hydroxide resulted in cis‐diamino‐diiodoplatinum II1 (3). Reaction of (3) with 1,1‐[1‐14C]cyclobutanedicarboxylic acid dipotassium salt in the pressence of silver nitrate resulted in the title compound (4).
The synthesis of carbon‐14 labeled 1‐(4,8‐dimethyl‐8‐methoxynonyl)‐4‐(1‐methylethyl)benzene
Authors: Aguinaga Guillermo M. , Dinizo Stephen E. 
Published: October 2006

AbstractThe title compound, uniformly labeled with carbon‐14 in the benzene ring, was prepared by Wittig reaction of 4‐isopropyl‐benzaldehyde‐14C ring (U) with 3,7‐dimethyl‐7‐methoxyoctylidene‐tripehylphosphrane followed by catalytic hydrogenation of the resulting mixture of olefins. A second route to the title compound, based on alkyllithium chemistry, was demonstrated using unlabeled intermediates. Attempted preparation of the title compound via the Horner‐Emmons modification of the Wittig reaction was unsuccessful.
Preparation of methyl 8c,11c‐eicosadienoate‐17,17,18,18‐d4, methyl 8c,11c,14c‐eicosatrienoate‐17,17,18,18‐d4 and methyl 5c,8c,11c‐eicosatrienoate‐17,17,18,18‐d4
Authors: Adlof R. O. , Emken E. A. 
Published: October 2006

AbstractMethyl 8c,11c‐eicosadienoate, methyl 5c,8c,11c‐eicosatrienoate and methyl 8c,11c,14c‐eicosatrienoate (all 17,17,18,18‐d4) were prepared in multi‐gram quantities for human metabolism studies. The deuterium atoms were incorporated by reduction of the appropriate acetylenic tetrahydropyranyl (THP) ethers with (Ph3P)3RhCl and deuterium gas. The THP ethers were converted to the iodides with H3PO4/P2O5/KI. The deuterium‐labelled fatty acid methyl esters were then synthesized from the alkyl iodide‐d4 via a series of acetylenic coupling reactions with the last double bond generated by the Witting reaction. Acetylenic bonds were reduced to olefinic bonds by use of Lindlar's catalyst. Both 8,11‐20:2 and 5,8,11‐20:3 were synthesized from the same 8‐carbon‐d4 starting fragment. The 8,11‐20:2 isomer was prepared in a 10‐step synthesis in 19% overall yield, the 5,8,11‐20:3 in 12 steps (18% overall yield) and the 8,11,14‐20:3 isomer in 12 steps with an overall yield of 10%. Trans isomers were removed by silver resin chromatography. The 8,11‐20:2, 5,8,11‐20:3 and 8,11,14‐20:3 compounds had isotopic purities of 91‐97%.
Syntheses of model oligosaccharides of biological significance. 8. A synthesis of a specifically deuterated 2‐propyl 3,6‐DI‐O‐[α‐D‐mannopyranosyl]‐β‐D‐mannopyranoside
Authors: Dime David S. , Rachaman Eliezer , Dime Charles E. , Grey Arthur A. , Carver Jeremy P. , Krepinsky Jiri J. 
Published: October 2006

AbstractThe title trisaccharide has been synthesized containing a 3‐deuterated central mannopyranosyl unit and 2,3,4,6,6′‐pentadeuterio mannopyranosyl units in both arms. 2‐Propyl 2‐O‐benzyl‐4,6‐O‐benzylidene‐3‐deuterio‐β‐D‐ mannopyranoside was obtained by stereoselective deuteride reduction of the corresponding 3‐oxo derivative and was reacted with 2,3,4,6,6′‐penta‐deuterio‐α‐D‐mannopyranosyl bromide. The disaccharide obtained was glycosylated with another equivalent of the same bromide after hydrolysis of the benzylidene group. This sequence led to the title compound after deblocking of all the hydroxyl groups. The 2,3,4,6,6′‐pentadeuterio mannopyranosyl bromide was obtained by a reaction sequence starting with a controlled deuterium exchange in deuterium oxide over Reney nickel catalyst of methylα‐D‐manno‐pyranoside, followed by acetolysis and purification via the corresponding ortheoster. The latter compound gave the bromide on reaction with trimethylesily bromid.
Synthesis of methyl 3‐oxo‐4,4‐dimethylpentanoate‐1,3‐14C
Authors: Sieving Paul 
Published: October 2006

AbstractA description of the preparation of methyl 3‐oxo‐4,4‐dimethylpentanoate‐1,3‐14C. The Grignard reagent prepared from 2‐chloro‐2‐methylpropane is carbonated with 14CO2 and the resulting trimethylacetic acid treated with methyllithium. 3,3‐Dimethyl‐2‐butanone is treated with NaNH2, the resulting enolate is carbonated with 14CO2, and this ketoacid treated immediately after workup with excess diazomethane.
Synthesis of oxygen‐18 isotope labeled amino acids and dipeptides and its effects on carbon‐13 NMR
Authors: Ponnusamy E. , Jones C. C. , Fiat D. 
Published: October 2006

AbstractOxygen‐18 isotope labeled at the carboxyl group of glycine, L‐alanine and L‐proline were synthesized by acid catalyzed exchange or acid hydrolysis of respective methyl ester derivatives of amino acids in HC1/H218O. Quantitative enrichment of glycine was achieved by the acid hydrolysis of amino acetonitrile in H218O. In order to conserve the isotopic enrichment [18O] dipeptides were synthesized by solid phase method. [18O] isotope effects on [13C] NMR of carboxylic carbon of amino acids and carbonyl carbon of peptides was observed. The [18O] isotopic shifts observed for the carboxylic carbon of singly and doubly [18O] labeled amino acids showed that the [18O] isotope effect is additive.
Synthesis of 2R, 4′R, 8′R‐α‐tocopherols selectively labelled with deuterium
Authors: Ingold K. K. , Hughes L. , Slaby M. , Burton G. G. 
Published: October 2006

AbstractNine deuterium‐labelled α‐tocopherols having the natural, 2R,4′R,8′R, stereochemistry have been synthesized for study by 2H NMR of the orientation and dynamics of natural α‐tocopherol in a phospholipid bilayer.
A new route to [5α,6α‐3H]androst‐16‐en‐3‐one
Authors: Rómer J. , Wagner H. 
Published: October 2006

AbstractA new simple synthesis of the boar pheromone [5α, 6α‐3H]‐androst‐16‐en‐3‐one with a specific activity of about 50 Ci/mmol and a radiochemical purity >99% is described.
Synthesis of 1‐14C‐(1S, 4S)‐N‐methyl‐4‐(3,4‐dichlophenyl)‐1,2,3,4‐tetrahydro‐1‐naphthalenamine L‐mandelate (1‐14C‐sertraline mandelate)
Authors: Welch Willard M. , Viveiros Dawn M. 
Published: October 2006

AbstractThe preparation of the title compound, a selective 5‐HT uptake blocker with potential antidepressant properties in man, is described. The labelled material with a specific activity of 0.7 mCi/mmol, was synthesized in 7 steps from K14CN in 6.5% radiochemical yield.
Synthesis of glycolic acid‐1‐14C of high specific activity a facile method of conversion of traces of alkali cyanide‐14C
Authors: Ramamurthy T. V. , Viswanathan K. V. 
Published: October 2006

AbstractA simple procedure is described which efficiently converts traces of 14C labelled cyanide present as a dilute solution into glycolic acid‐1‐14C with more than 85% radiochemical recovery and of high specific activity.
Synthesis of 14C‐labelled DDD isomers of high specific activity
Authors: Lindholm Ann , Klasson‐Wehler Eva , Wehler Thomas , Bergman Ake 
Published: October 2006

AbstractThree major DDD isomers, o,p'‐DDD, m,p'‐DDD and p,p'‐DDD, 14C‐labelled in the para‐chlorophenyl ring, have been synthesized. The DDD products were obtained in isotopic yields ranging from 42% to 58% and were of high specific activities; 31 mCi/mmol (o,p'‐DDD; m,p'‐DDD) and 19,8 mCi/mmol (p,p'‐DDD). A minor amount of 14C‐labelled o,m'‐DDD was also isolated. 400 MHz 1H NMR data of the three major DDD isomers and o,m'‐DDD were obtained.
The preparation of a carbon‐11 labelled analgesic — [N‐methyl‐11C]meptazinol
Authors: Turton David R. , Luthra Sajinder K. , Pike Victor W. , Kensett Malcolm J. 
Published: October 2006

AbstractA procedure for labelling the novel analgesic, meptazinol [(+)1‐methyl‐3‐ethyl‐3‐(m‐hydroxyphenyl)tetrahydroazepine], with the positron‐emitting radionuclide, carbon‐11 (t1/2 = 20.4 min) has been developed in order to permit the pharmacokinetics of this analgesic to be studied in man. The procedure involves the reaction of [11C]iodomethane, itself produced from cyclotron‐produced [11C]carbon dioxide, with normeptazinol in ethanol at 100°C for 5 min, evaporation of any unreacted [11C]iodomethane, purification by HPLC and removal of solvent. Subsequent solubilisation of the radioactive product in ethanol plus isotonic saline and sterilisation by filtration produces a safely‐injectable solution of [N‐methyl‐11C]meptazinol in 14% radiochemical yield (from cyclotron‐produced [11C]carbon dioxide, decay‐corrected). The specific activity of the product is up to 7.4 GBq/μmol at the end of radiosynthesis (40 min from the end of radionuclide production). Preparations have been shown to be radiochemically pure and to be free of normeptazinol by analytical HPLC and TLC. That the radioactive product is [N‐methyl‐11C]meptazinol has been unequivocally demonstrated by co‐inclusion of 13C‐enriched iodomethane in the radiosynthesis and examination of the product by broad‐band proton‐decoupled Fourier transform 13C‐NMR spectroscopy.
Synthesis of iodine‐125 labeled phorbol ester‐a useful gamma‐emitting analog of 12‐o‐tetradecanoylphorbol‐13‐acetate
Authors: Mishra Nrusingha C. , Estensen Richard D. , Abdel‐Monem Mahmoud M. 
Published: October 2006

AbstractIodine‐125 labeled analog of 12‐O‐tetradecanoylphorbol‐13‐acetate (TPA) was obtained by heating the iodine substituted analog of TPA in acetone with sodium [125I] iodide. The iodine substituted analog of TPA, 12‐O‐(12′‐iodododecanoyl)phorbol‐13‐acetate (IPA), was synthesized from phorbol by a three step reaction sequence. The structure of IPA was confirmed by high resolution proton magnetic resonance, fast atom bombardment mass spectrometry (FAB) and chemical ionization mass spectrometry (CIMS).The [125I]‐IPA was purified by normal phase flash column chromatography. The product had 99% radiochemical purity and specific activity of Ca. 2.7Ci/mmol.
Synthesis of [6‐2H] and [6‐3H]fecapentaene‐12
Authors: Kassaee Mohamad Z. , Kingston David G. I. 
Published: October 2006

AbstractThe title compounds (6 and 9) were prepared by exchange of the α‐protons of (E,E)‐2,4,‐heptadienyldiphenylphosphine oxide (2) with either 2H2O or 3H2O, followed by condensations with (E,E)‐5‐[2,3‐bis(t‐butyldimethylsilyl) oxy]‐propoxy‐2,4‐pentadienal (4) and deprotection.
Carrier‐free astatination of steroid hormones
Authors: Pillai K. K. R. , McLaughlin W. W. , Lambrecht R. R. , Bloomer W. W. 
Published: October 2006

AbstractThe alpha emitting radiohalogen 211At has potential use as a radiotherapeutic agent when linked to biologically active molecules. The range of compounds which may be astatinated is limited by relative lack of knowledge of organoastatine syntheses. The production of astatovinyl steroids was carried out via electrophilic substitution of tri‐n‐butylstannylvinyl steroids with astatide in the presence of mild oxidizing agents. The astatinated steroids are synthesized rapidly and in carrier‐free fashion yielding compounds of high radiochemical purity.
No‐carrier‐added radiobromination via the gattermann reaction. — Synthesis of 75Br‐ and 77Br‐bromperidol —
Authors: Suehiro Makiko , Yokoi Fuji , Nozaki Tadashi , Iwamoto Masako 
Published: October 2006

AbstractThe Gattermann reaction was applied to the no‐carrier‐added radiobromination of bromperidol. The synthesis with diazotized precursor, no‐carrier‐added 75Br‐ or 77Br‐, and copper powder proved to give the radiobrominated neuroleptic drug in high radiochemical yield of 60 ‐ 70%, and in high specific activity (∼5 Ci/umole). The radiobromination also proved to be regioselective. In the reaction, the copper catalyst was observed to play an important role.Formation of unlabeled by‐products due to stable chlorine or bromine contamination in the reaction mixture was also studied by neutron activation analysis. Removal of such undesirable halogen nuclides and separation of the unavoidably‐formed chlorinated coupound from the radiobrominated bromperidol is discussed.