bluuebunny/crossref_metadata_2025_split huggingface dataset:
An improved synthesis of [15N] 16‐doxyl stearic acid
Authors: Joseph Joy , Lai Ching‐San 
Published: October 2006

AbstractAn improved method for the synthesis of [15N] 16‐Doxyl stearate, a fatty‐acid spin label, is reported. The method requires only one mole of [15N] 2‐amino‐2‐methyl propanol per mole of methyl keto stearate with an overall yield of about 50%. In contrast, the previous method produced only 1‐3% yield. The great improvement in yield was achieved mainly through the reduction of reaction volume which increases the reaction rate by the law of mass action.
Synthesis of 14C‐labeled 3‐{[1‐ethoxycarbonyl‐3‐phenyl‐(1S)‐phenyl‐(1S)‐propyl]amino}‐2,3,4,5‐tetrahydro‐2‐oxo‐1H‐1‐(3S)‐benzazepine‐1‐acetic acid hydrochloride ([14C]CGS 14824A)
Authors: Chaudhuri Naba K. , Patera Russell , Markus Bohdan , Sung Ming‐Sang 
Published: October 2006

AbstractThe title compound, CGS 14824A, was synthesized with a 14C‐label in the azepine ring in 14 steps starting with 1‐bromo‐3‐phenylpropane (1) and K14CN in an overall yield of 1.31%. The reaction of 1 with K14CN yielded the nitrile 2 which upon hydrolysis followed by ring closure gave α‐tetralone‐1‐14C (4). Bromination of 4 followed by oxime formation gave the bromo oxime 5, which upon Beckmann rearrangement by acid treatment yielded the ring expansion product 6. The bromine atom of 6 was then replaced by an azido group, and an acetic ester side chain was introduced at the nitrogen atom. Catalytic reduction of the azido compound 8 gave a mixture of epimeric amino esters which was resolved by salt formation with L‐tartaric acid. The negatively rotating isomer was then reacted with 4‐phenyl‐2‐oxo‐butanoate in presence of sodium cyanoborohydride to give a mixture of diastereoisomers which were separated as their benzyl esters by chromatography. The major isomer was then converted to labeled CGS 14824A.
Synthesis of deuterated optically active verapamil and gallopamil, and of N‐13C‐methyl‐verapamil
Authors: Theodore Louis J. , Nelson Wendel L. 
Published: October 2006

AbstractDeuterated (‐)‐verapamil, (2S)‐(‐)‐2‐(2,5,6‐2H3‐3,4‐dimethoxyphenyl)‐2‐isopropyl‐5‐[(2,5,6‐2H3‐3,4‐dimethoxyphenethyl)methylamino]valeronitrile, and its analog (‐)‐2H5‐gallopamil, (2S)‐(‐)‐2‐(2,6‐2H2‐3,4,5‐trimethoxyphenyl)‐2‐isopropyl‐5‐[(2,5,6‐2H3‐3,4‐dimethoxyphenethyl)methylamino]valeronitrile, were prepared. (‐)‐Gallopamil readily incorporated five atoms of deuterium into the available positions in the aromatic rings. (‐)‐2H6‐Verapamil was prepared from ring trideuterated 3,4‐dimethoxyphenylacetic acid and (2S)‐(+)‐triphenyl‐methoxy‐2‐[(methanesulfonyl)oxy]propane. Three additional atoms of deuterium were incorporated into the aromatic ring of the N‐methyl‐3,4‐dimethoxyphenethylamine moiety incorporated as the the short N‐alkyl side chain. N‐13C‐Methylverapamil was prepared from N‐13C‐methyl‐3,4‐dimethoxyphenethylamine.
Synthesis of 14C‐labeled perfluorooctanoic and perfluorodecanoic acids; purification of perfluorodecanoic acid
Authors: Reich Ieva L. , Reich Hans J. , Menahan Lawrence A. , Peterson Richard E. 
Published: October 2006

AbstractPerfluoro‐n‐octaboic acid (PFOA) and perfluoro‐n‐decanoic acid (PFDA), two widely used industrial products, have been synthesized with 14C‐labeling in the C‐1 position. The carboxyl labeled materials were prepared in 48% and 53% yield by carbonation of perfluoroheptyllithium and perfluorononyllithium at −100°C. An efficient chemical method for purification of PFDA was also developed. Treatment of commercial PFDA with refluxing potassium hydroxide solution resulted in removal of the mono and diprotio impurities to give 99% pure PFDA.
Synthesis of deuterium labelled penicillamine and its use for the assignment of the 1H NMR spectra of two cyclic enkephalin analogs
Authors: Mosberg Henry I. , Omnaas John R. , Ramalingam Kondareddiar , Woodard Ronald W. 
Published: October 2006

AbstractThe synthesis of D,L‐[4,4′‐2H6]penicillamine (D,L‐[2H6]Pen) and its incorporation into the cyclic, disulfide‐containing peptides, [D‐Pen2,D‐[2H6]Pen5]enkephalin (DPDPE) and [D‐Pen2,L‐[2H6]Pen5]enkephalin (DPLPE), both highly δ opioid receptor‐selective analogs, are described. The deuterium‐labelled peptides allowed the assignment of the four Pen methyl group resonances in each of the corresponding unlabelled peptides to specific Pen residues.
Synthesis of DL‐[7‐14C]indospicine and DL‐2‐amino[7‐14C]pimelic acid
Authors: Wieczorkowska Elzbieta , Hegarty Mervyn P. 
Published: October 2006

AbstractA new method of synthesis of DL‐[7‐14C]indospicine and DL‐2‐amino‐[7‐14C]pimelic acid and their nonradioactive equivalents is reported. The combined radiochemical yield of both compounds, starting from potassium [14C]cyanide was 15.3%. Indospicine was isolated as the flavianate.
Preparation of tritium‐labeled diosgenin, esmilagenin and tigogenin
Authors: Rabinowitz Joseph L. , Juarez‐Oropeza  , Zagoya Juan C. Diaz 
Published: October 2006

AbstractThe synthesis of 3H ‐diosgenin, 3H ‐esmilagenin and 3H ‐tigogenin (three potential hypocholesterolemic agents) was accomplished by low pressure hydrogenation of commercial (Sigma D 1634) diosgenin with 3H ‐gas. The mixture of 3H materials obtained was separated by silica gel G‐60 column chromatography by use of a benzene: ethyl acetate (8:2 v/v) solution. Purification of each sapogenin was by TLC chromatography.
Preparation of [3H]‐prazosin
Authors: Dezhu Wu , Xiuzhen Qi , Chunfang Hou , Yading Sun 
Published: October 2006

AbstractThe synthesis of the bromoprazosin, in which bromination and acylation of furoic acid were completed by means of very simple method was described. The reductive catalyzed debromination with tritium gas afforded the (3H)‐prazosin. Its specific activity and radiochemical purity were 22.6 Ci/mmol and 98% respectively.
Preparation of carbon 14‐labelled “Spy Dust” 5‐(4‐nitrophenyl)‐2,4‐[5‐14C]pentadienal, (NPPD)
Authors: Brown Susan I. , Rotert Gary A. , Lamontagne Maurice P. 
Published: October 2006

AbstractPreparation of carbon 14‐labelled “Spy Dust”, 5‐(4‐nitrophenyl)‐2,4‐[5‐14C]pentadienal is described. The facile synthesis of 4‐nitro[formyl‐14C]benzaldehyde from 1‐iodo‐4‐nitrobenzene by reaction with K14CN/CuCN, followed by reduction with diisobutylaluminum hydride provided this key intermediate in 50% yield. Subsequent treatment with the resonance‐stabilized ylide, formylmethylenetriphenylphosphorane, afforded the title compound.
Synthesis of 123I‐ and 131I‐labelled derivatives of low‐density lipoprotein for radiopharmaceutical use
Authors: Moerlein S. S. , Dalal K. K. , Yano Y. 
Published: October 2006

AbstractThe syntheses of two analogues of low‐density lipoprotein (LDL) labelled with 123I or 131I was optimized for radiopharmaceutical application. Rabbit LDL was employed due to its usefulness in pre‐clinical experimentation, although the parameters which were optimized also pertain to human LDL. LDL was iodinated directly with exchange‐labelled [123I]ICI to produce injectable [123I]LDL in 40% radiochemical yield within 30 min. A derivatized version of LDL, [123I]TC‐LDL, was produced in about 30% radiochemical yield within 75 min by radioiodination of tyramine‐cellobiose (TC) via in situ oxidation of 123I− followed by cross‐linking to LDL using cyanuric chloride. Quality control tests indicated that both radioiodinated LDL and TC‐LDL were very similar in character to the native LDL molecule.
Synthesis of carbon‐14 labelled spiro‐piperidyl‐rifamycins (LM 118) and rifabutin (LM 427)
Authors: Fontana Erminia , Giarda Silvio , Vioglio Sergio , Vicario Gian Piero 
Published: October 2006

AbstractTwo syntheses of radiolabelled spiro‐piperidyl‐rifamycins are described.

. A five steps synthesis (Scheme 1) was performed to give 4‐deoxo‐3,4‐[2‐spiro‐(N‐[14C]methyl‐4‐piperidyl)]‐(1H)‐imidazo‐(2,5‐dihydro)‐rifamycin S ([14C]LM 118), in an overall radiochemical yield of ∼ 20%, 98% radiochemically pure and with a specific activity of 440 MBq/mmol (11.9 mCi/mmol) starting from [14C]methyl iodide 1.
. A three steps synthesis (Scheme 2) was performed to give 4‐deoxo‐3,4‐[2‐spiro‐(N‐2‐methyl[1‐14C]propane‐4‐piperidyl)]‐(1H)‐imidazo‐(2,5‐dihydro)‐rifamycin S ([14C] rifabutin) in an overall radiochemical yield of ∼38%, 97% radiochemically pure with a specific activity of 1.27 GBq/mmol (34.32 mCi/mmol). 1‐(2‐Methyl[1‐14C]propanoyl)‐piperazin‐4‐one ethylene ketal was employed as starting material.
Synthesis of tritium and deuterium labeled 8‐N‐n‐butyl‐N‐methylamino‐8‐(3‐hydroxyphenyl)‐1,4‐dioxaspiro[4,5]decane hydrochloride
Authors: Hsi Richard S. P. , Kurtz Richard R. , Moon Malcolm W. 
Published: October 2006

AbstractThe title compound, a 4‐amino‐4‐arylcyclohexanone derivative with central analgesic activity, was labeled with tritium at the C‐7 and C‐9 positions. Deuterium labeled intermediates were used as models for developing isotope exchange and synthetic procedures. Deuterium and tritium labeled title compounds were obtained in five steps with overall yields of 18‐22% from 1,4‐dioxaspiro[4,5]‐decan‐8‐one and 3‐bromophenol.
Synthesis of 5‐amino[carboxyl‐14C]salicylic acid
Authors: Jørgensen Ole , Petersen Susanne , Carlsen Lars 
Published: October 2006

AbstractImprovements have been made to the synthesis of 5‐aminosalicylic acid (5‐ASA) in order to make it applicable for the small‐scale synthesis of 5‐amino[carboxyl‐14C]salicylic acid.
Synthesis of 14C‐ and 3H‐labeled fluoxetine, a selective serotonin uptake inhibitor
Authors: Robertson David W. , Krushinski Joseph H. , Wong David T. , Kau Don 
Published: October 2006

AbstractFluoxetine (N‐methyl‐γ‐(4‐(trifluoromethyl)phenoxy)benzenepropanamine) is a potent, highly selective serotonin uptake inhibitor that is useful in treating a variety of major psychiatric derangements. We have synthesized this compound in 14C‐ and 3H‐labeled forms. The tritium label was introduced in the final step by catalytic dehalogenation of the brominated fluoxetine precursor 6. Reaction conditions could be controlled such that catalytic hydrogenolysis of the labile C‐O benzylic bond was minimized. Following HPLC purification, [3H]‐fluoxetine was obtained in a state of high radiochemical purity (98%) and specific activity (20.4 Ci/mmol). The 14C‐label was introduced in the final step via a nucleophilic aromatic substitution reaction between the sodium salt of α‐(2‐(methylamino)ethyl)benzenemethanol and uniformly ring‐labeled p‐chlorobenzotrifluoride. Following purification by flash chromatography, [14C]‐fluoxetine was obtained in 98.3% radiochemical purity with a specific activity of 5.52 mCi/mmol.
Syntheses of deuterium labeled bile alcohols
Authors: Kihira Kenji , Kosaka Daisaku , Une Mizuho , Hiraoka Toshihito , Kajiyama Goro , Hoshita Takahiko 
Published: October 2006

AbstractThe following major bile alcohols, identified in urine of healthy humans and in bile and urine of patients with cerebrotendinous xanthomatosis, were synthesized as internal standards for mass spectral analyses: [26,27‐D6]5β‐cholestane‐3α,7α,12α,25‐tetrol, [26,27‐D6](23S)‐5β‐cholestane‐3α,7α,12α,23,25‐pentol, [27‐D3]5β‐cholestane‐3α,7α,12α,25,26‐pentol, and [2,4‐D4]27‐nor‐5β‐cholestane‐3α,7α,12α24,25‐pentol.
Synthesis of a deuterium labeled variant of the rat hepatocarcinogen, methapyrilene
Authors: Kammerer R. Craig , Kloc Kenneth 
Published: October 2006

AbstractMethapyrilene, I, once a commonly found antihistamimic drug, has been synthesized with four deuterium labels, three of which are on the thiophene ring. Initially, thiophene was deuterated by solvolysis of the tetramercuric acetate‐derivative with deuterium chloride. Carbonylation of the thiophene ring at the 2‐position, by the addition of dimethylformamide to the 2‐lithio‐derivative, gave [3,4,5‐d3] thiophene‐2‐carboxaldehyde. Condensation of this aldehyde with 2‐aminopyridine was followed by reduction of the resulting imine with sodium borodeuteride to yield the N‐([3,4,5‐d3]‐2‐thienyl[d]‐methylene)‐2‐aminopyridine, VIII. Alkylation of the lithium salt of VIII with dimethylaminoethylchloride gave N, N‐dimethyl‐N'‐[2‐pyridyl]‐N'‐([3,4,5‐d3]‐2‐thienyl‐[d]methylene)‐1,2‐ethane diamine, I, in good yield. Combustion analysis, 500 mHz NMR, and mass spectrometry confirmed the identity of the product which will be useful for metabolic studies.
Enhanced incorporation of nonhydrolyzable tritium in GnRH and TRF by catalytic exchange labeling
Authors: Oehlke J. , Mittag E. , Tóth G. , Bienert M. , Niedrich H. 
Published: October 2006

AbstractGonadotropin releasing hormone (GnRH), D‐Phe6‐GnRH and thyrotropin releasing factor (TRF) were tritiated by direct catalytic exchange using Rh/Al2O3 + HT under conditions which lead in model deuterations of Nα‐acetylhistidine amide to a high incorporation of deuterium into position 5 of the histidine ring. Specific activities up to a range of 400 GBq/mmol in form of nonhydrolyzable tritium are attainable after removal of the label incorporated into position 2 of the histidine ring. A crucial reason for diminished specific activities was found to be a catalystmediated hydrogen transfer between the peptides and traces of water, contained in the reaction mixture, competing with the tritiation.
A simple apparatus for reductive labelling with isotopic hydrogen gas at atmospheric pressure
Authors: Lockley William J S 
Published: October 2006

AbstractA simple apparatus is described for the generation of isotopic hydrogen gas by acid‐catalyzed hydrolysis of sodium borotritide or borodeuteride. The apparatus may be conveniently utilized for isotopic hydrogen reductions of from 20 μmol to 1 mmol scale.
Synthesis and biological evaluation of p,p′‐dideuteriophenytoin
Authors: Poupaert Jacques H. , Guiot Pierre , Dumont Pierre 
Published: October 2006

AbstractA reaction sequence is described to synthesize p,p′‐dideuteriophenytoin in three steps from commercially available starting materials. The deuterium content at best reached 99.2% as measured by mass spectrometry. For materials with isotopic content up to 95%, excellent agreement was found between the data obtained by mass spectrometry and 13C‐nuclear magnetic resonance operated in a NOE‐suppression mode. p,p′‐Dideuteriophenytoin was evaluated comparatively with phenytoin and p‐deuteriophenytoin in the maximal electroshock test. While all three compounds exhibited a high degree of antiepileptic activity, none of them demonstrated significant superiority over the others.
Synthesis of D/D‐norepinephrine‐ (phenyl‐U‐13C)
Authors: Weisz Adrian , Markey Sanford P. 
Published: October 2006

AbstractThe synthesis of phenyl‐U‐carbon‐13 labelled D,L‐norepinephrine from catechol‐U‐13C in three steps is described. In the first step, the Friedel‐Crafts acylation of the labelled part with N‐phthaloylglycylchloride yielded the aromatic ketone adduct. Subsequent hydrolysis and catalytic hydrogenation produced the desired product in a 5% overall yield.
Efficient syntheses of (±) [2‐2H2]mevalonolactone and (±) [2‐2H2]homomevalonolactone
Authors: Banerji Asoke , Kalena Govind P. 
Published: October 2006

AbstractEfficient syntheses of (±) [2‐2H2]mevalonolactone and (±) [2‐2H2]homomevalonolactone involving condensations of lithiotrimethylsilyl [2‐2 H2]acetate with appropriate 3‐oxo‐alcohols are described. Regiospecificity of the label was established by NMR spectroscopy.
Synthesis of 14C‐ and 2H‐labeled (3S)‐1‐benzyl‐3‐pyrrolidinyl methyl (4S)‐2,6‐dimethyl‐4‐(m‐nitrophenyl)‐1,4‐dihydropyridine‐3,5‐dicarboxylate hydrochloride (YM‐09730‐5), a potent calcium antagonist
Authors: Arima Hideki , Tamazawa Kazuharu , Takeuchi Makoto 
Published: October 2006

AbstractA potent and long acting calcium antagonist YM‐09730‐5, (3S)‐1‐benzyl‐3‐pyrrolidinyl methyl (4S)‐2,6‐dimethyl‐4‐(m‐nitrophenyl)‐1,4‐dihydropyridine‐3,5‐dicarboxylate hydrochloride (7a·HCl), was labeled with carbon‐14 and deuterium. The labeled materials were prepared by either the cyclizing Michael addition of 3‐aminocrotonate (5c) to benzylidene acetoacetate (6) or the modified Hantzsch reaction using m‐nitrobenzaldehyde, aminocrotonate(5a) and acetoacetate (3b). The 14C‐labeled material (7c·HCl) was synthesized from methyl [3‐14C]acetoacetate (4c) in a 32.0% radiochemical yield, at a specific activity of 60.9 mCi/mmol. The deuterium labeled material (7b·HCl) was synthesized from 1‐benzyl‐3‐hydroxypyrrolidine‐d4 (2b) which was obtained by the reduction of succinimide (1) with LiAlD4.
N.C.A. 18F‐fluoroacylation via fluorocarboxylic acid esters
Authors: Block Dirk , Coenen Heinz Hubert , Stöcklin Gerhard 
Published: October 2006

AbstractThe preparation and introduction of fluoroacyl moieties as prosthetic groups is described for n.c.a. labelling with fluorine‐18. Activation by the aminopolyether 2.2.2./K2CO3 complex was used for the nucleophilic 18F‐exchange in α‐substituted acid esters. Increasing yields were found in the sequence: iodo << chloro < tosyloxy < bromo. The methylester of α‐bromopropionic acid proved to be the best precursor for acylation. The [2‐18F]fluoropropionic acid methylester was prepared with radiochemical yields of > 90% within 10 minutes. It reacted effectively with primary alcohols in the presence of 3% methane sulfonic acid. Using n‐butylamine as model compound and O.1% NH4Cl as acid in aqueous solution, n.c.a. N‐fluoroacylation was also performed with > 80% radiochemical yield. This reaction is relevant to 18F‐labelling of biomolecules such as peptides.
Enantioselective synthesis of 11C‐labeled phenylethanolamine
Authors: Maeda Minoru , Nishimura Shuichi , Fukumura Toshimitsu , Kojima Masaharu 
Published: October 2006

AbstractNo‐carrier‐added [1‐11C]phenylethanolamine was prepared by the oxynitrilase‐catalyzed addition of hydrogen [11C]cyanide to benzaldehyde followed by reduction of the [11C]cyanohydrin. Radiochemical yields of 2‐4% at end‐of‐synthesis were obtained in a preparation time of 50‐60 min from the end of hydrogen [11C]cyanide production. The enantiomeric composition was determined through its conversion to the diastereomeric Mosher amide‐esters; the enantiomeric purity of the [11C]phenylethanolamine produced via NaBH4‐CoC12 reduction was 60% e.e. (R/S = 80/20) while that prepared through boran‐THF complex reduction was 80% e.e. (R/S = 90/10).
Synthesis of 13 C labelled unsymmetrically substituted maleic anhydrides
Authors: Breau L. , Kayser M. M. 
Published: October 2006

AbstractMethylmaleic (citraconic) and ethoxymaleic anhydrides labelled with 13C at C‐4, and phenylmaleic anhydride labelled at C‐1 were prepared in excellent yields from inexpensive starting materials. The methodology described here can be applied in a synthesis of a variety of substituted maleic anhydrides.
Synthesis of 5‐,6‐, and 7‐deutero sparteines
Authors: Meese Claus O. , Ebner Thomas 
Published: October 2006

AbstractKinetically controlled1H/2H exchange at carbon atom 5 of (‐)‐1,6‐dehydrosparteinium monoperchlorate (3a) followed by sodium borohydride or sodium borodeuteride reduction of the iminium double bond gave optically active 5,5‐(2H2)‐sparteine (1b) and 5,5,6‐(2H3)‐sparteine (1c), respectively. Under thermodynamic control a third deuterium atom was incorporated into3at carbon atom 7. Borohydride reduction or rapid re‐exchange followed by reduction lead to the novel sparteine analogues 5,5,7‐(2H3)‐sparteine (1d) and 7‐(2H)‐sparteine (1e). The title compounds have been prepared in 76 to 83 % yield and 89 to 97 % isotopic purity.
[14C] – radiolabeling of {[trans‐(8β)]‐6‐methyl‐1‐(1‐methylethyl) ergoline‐8‐carboxylic acid, 4‐methoxycyclohexyl ester (Z)‐2‐butenedioate [(1:1)]. A potent and selective 5ht2‐receptor antagonist
Authors: Marzoni Gifford , Wheeler William J. , Garbrecht William L. 
Published: October 2006

Abstract[14C]‐Labeled {[trans‐(8 β)]‐6‐methyl‐1‐(1‐methylethyl)ergoline‐8‐carboxylic acid, 4‐methoxycyclohexyl ester (Z)‐2‐butenedioate (1:1)} (LY281067) (10) was synthesized from unlabeled 6‐methyl‐1‐(1‐methylethyl)ergoline‐8‐carboxylic acid (2). The [14C] label was introduced into the carboxyl group attached to the 8 position of the ergoline nucleus. This site is stable to metabolism. The synthesis involves removal of the unlabeled carboxyl group from 2 and subsequent reinsertion of a [14C]‐labeled carboxyl group into the same position. The radiolabel is not introduced until near the end of the synthesis which allows for ease of handling and scale‐up of intermediates.
Preparation and characterization of 2‐deoxy‐2‐[18F] fluoro‐D‐galactose
Authors: Oberdorfer Franz , Traving Birgitt‐C. , Maier‐Borst Wolfgang , Hull William E. 
Published: October 2006

Abstract2‐Deoxy‐2‐[18 F] fluoro‐D‐galactose was prepared using gaseous [18F]acetyl hypofluorite or [18F]F2 and tri‐O‐acetyl‐D‐galactal as substrate. The product was obtained in a surprisingly high epimeric purity (>90%), even with [18F]F2 as fluorinating reagent, as demonstrated by HPLC and high‐resolution 1H‐ and 19F‐NMR spectroscopy. This is the first report of a highly stereoselective reaction using molecular fluorine in a polar protic solvent. Epimerization at C‐3 of galactal led to α‐2‐deoxy‐2‐fluoro‐D‐idose and α‐2‐deoxy‐2‐fluoro‐D‐gulose as minor products. A simple apparatus for a partially remote‐controlled preparation of 2‐deoxy‐2‐[18F]fluoro‐D‐galactose is also described.
Synthesis of specific labelled [methyl‐14C]sarin
Authors: Chang Sin‐Ren A. , Riggio Gaetano , Hopff Wolfgang H. , Waser Peter G. 
Published: October 2006

AbstractSynthesis of specific labelled [methyl‐14C]sarin. The synthesis of labelled [methyl‐14C]sarin, [14C]methylphosphonofluoridic acid 1‐methylethyl ester, was accomplished by another approach as for nonlabelled sarin in a tele‐conducted reaction vessel. The purity was estimated by IR, GC, and GC‐MS and the stability in different media was examined.
Synthesis of (5‐methyl‐2‐oxo‐1,3‐dioxol‐4‐YL)methyl 7‐[D‐O‐(L‐alanyl)[β‐14C]mandelamido]‐3‐[[(5‐methyl‐1,3,4‐thiadiazol‐2‐YL)thio]methyl]‐3‐cephem‐4‐carboxylate and its active compound
Authors: Nishizawa Susumu , Matsui Hiroshi , Ohkubo Akio , Kakeya Nobuharu , Kiritani Reiko 
Published: October 2006

Abstract(5‐Methyl‐2‐oxo‐1,3‐dioxol‐4‐yl)methyl 7‐[D‐O‐(L‐alanyl)[β‐14C]‐mandelamido]‐3‐[[(5‐methyl‐1,3,4‐thiadiazol‐2‐yl)thio]methyl]‐3‐cephem‐4‐carboxylate (14C‐KY‐109) and its parent drug (14C‐KY‐087) were synthesized from D‐(‐)‐mandelic‐β‐14C acid prepared by optical resolution of DL‐(±)‐ mandelic‐β‐14C acid. The overall radiochemical yields were 16.2% for 14C‐KY‐087 and 49.6% for 14C‐KY‐109, based on D‐(‐)‐mandelic‐β‐14C acid. Both the products had radiochemical purities greater than 97% as measured by TLC.
Kit type labelling of [123I] metaiodobenzylguanidine
Authors: Dougan H. , Lyster D. M. , Vincent J. S. , Rihela T. 
Published: October 2006

AbstractWe have examined the labelling of [123I] MIBC by a Cu(I) catalyzed reaction in aqueous solution. We regularly obtained >99% radiochemical purity [123I] MIBC product and >97% radiochemical yield. At 100°C with 2 mg MIBG the radiochemical purity reached 85% at 2.5 min, 97% at 5 min and 99% at 10 min through 30 min. With 200 μg MIBG the reaction proceeded at roughly one tenth the former speed. Many details of technique were essential; the highlights were use of dry triturated reagents and the use of H2SO4 solvent. Neglect of proper procedure led to low radiochemical yields and 123I bound to apparatus. The procedure has been utilized with up to 1.0 mL 123I (0.1N NaOH) or 93 mCi 123I. A study of temperature dependence showed that the reaction proceeded readily, albeit more slowly at 20°C. The temperature coefficient at 100°C was estimated ∼1.7.