bluuebunny/crossref_metadata_2025_split huggingface dataset:
Radio‐ and fluorescence‐labelling of thapsigargin, a selective inhibitor of microsomal calcium‐ATPase
Authors: Andersen Annette , Lauridsen Annette , Br Christensen S. ØGger 
Published: October 2006

AbstractDebutanoylthapsigargin (2) labelled in the skeleton was prepared by stereoselective reduction of the ketone (3) obtained by oxidation of debutanoylthapsigargin. Butanoylation of 2 yielded thapsigargin 1. The use of sodium boro[3H]hydride as a reducing agent afforded labelled debutanoylthapsigargin with a specific activity of 22 Ci/mmol.A fluorescent analogue of thapsigargin (4a) was prepared by allowing 2 to react with N‐dansyl‐β‐alanine. Acetylation of 4a afforded a trisacetate (4c) the missing bioactivity of which allows it to be used as a negative control.
Synthesis and binding to striatal membranes of no carrier added I‐123 labeled 4′‐iodococaine.
Authors: Metwally S. A. M. , Gatley S. J. , Wolf A. P. , Yu D.‐W. 
Published: October 2006

AbstractAn 123I labeled cocaine analog, 4′‐[123I]iodococaine, has been prepared by oxidative destannylation of the tributyltin analog and shown to interact with cocaine binding sites in rat brain striatal membranes. It may thus be a suitable SPECT radiotracer for studies of the dopamine reuptake site in neurodegenerative diseases.
Preparation of tritium‐labelled dextran and inulin
Authors: Akulov G. P. , Kaminski Ju. L. , Korsakova N. A. , Kudelin B. K. 
Published: October 2006

AbstractTritiated dextran and inulin were prepared by both a catalytic solid state and a liquid phase isotope exchange with gaseous tritium. The liquid phase procedure is convenient for preparation of the polysaccharides with specific activities up to 5 mCi/g, while the solid state procedure allows specific activities up to 700 mCi/g.
Synthesis of [14C]‐labeled N‐tert‐butyl‐α‐phenylnitrone. A potential spin‐trapping agent
Authors: Angelini G. , Carnevaletti F. , Piccinini F. 
Published: October 2006

AbstractA single step synthesis of the [14C‐ring]‐N‐tert‐butyl‐α‐phenylnitrone (1) starting from the [14C‐ring] benzaldehyde is described. The product is obtained in high yield (90%) with a good level of purity.
A high yield microscale enzymatic synthesis and purification Of 14C‐Labeled Nicotinamide Adenine Dinucleotide Phosphate (NADP+)
Authors: Ronneberg Andre , Metz Gordon , Weld Richard , Roffey Peter , Craney Chris 
Published: October 2006

AbstractUniformly labeled (U) 14C nicotinamide adenine dinucleotide phosphate (NADP+) was synthesized by phosphorylating [U‐14C]nicotinamide adenine dinucleotide (NAD+) in the presence of immobilized NAD+ kinase. The 15 μCi (600 μL) synthesis consistently achieved yields between 80% and radiochemical purities greater than 95%. The [U‐14C]NADP+ was purified by high performance anion‐exchange chromatography using a gradient elution of ammonium bicarbonate. This procedure may be applicable to the synthesis of other charged, UV‐absorbing products of enzyme‐catalyzed reactions.
The synthesis of [14C]pantoprazole ‐ SK&F 96022Z. An H+/K+ ATPase inhibitor
Authors: Crowe A. M , Johnston C. E. A , Lawrie K. W. M , Saunders D 
Published: October 2006

AbstractPantoprazole 1, SK & F 96022Z, an H+/K+ ATPase inhibitor has been prepared, radiolabelled with carbon‐14, in two positions, for drug metabolism studies. [Benzimidazole‐2‐14C]Pantoprazole in 4 steps from potassium ethyl [14C]xanthate, and [pyridylmethyl‐14C]pantoprazole from cuprous [14C]cyanide in 8 steps. The overall radiochemical yields of these syntheses were 37.9% and 5.2% respectively.
An efficient method for synthesizing [d6]‐butadiene monoepoxide
Authors: Maples Kirk R. , Lane Jennifer L. , Dahl Alan R. 
Published: October 2006

AbstractEpoxides are known mutagenic and carcinogenic metabolites of alkenes. During current toxicological investigations in our laboratory, we have monitored in vivo epoxide levels using gas chromatography/mass spectroscopy isotope dilution assays. These assays require the use of deuterated analogues for the expected epoxide metabolites. To determine whether butadiene monoepoxide is formed in vivo following inhalation of 1,3‐butadiene, deuterated butadiene monoepoxide, a compound that is not commercially available, was needed. To meet this need, we developed a method using monoperoxyphthalic acid to synthesize [d6]‐butadiene monoepoxide from [d6]‐1,3‐butadiene with a reaction time of 50 min and a 94% yield.
Synthesis of some useful tritium labelled auxins
Authors: Buchman O. , Pri‐Bar I. , Shimoni M. , Azran J. 
Published: October 2006

AbstractThe synthesis of six useful auxins labelled with tritium is described. The following compounds were prepared: 3‐indoleacetic acid‐5‐3H (28.9 Ci‐1.07 TBq/mmol), 3‐indolebutyric acid‐5‐3H (7.3 Ci‐270 GBq/mmol), 1‐naphthylacetic acid‐4‐3H (27.6 Ci‐1.02 TBq/mmol), 2,4‐dichlorophenoxyacetic acid‐5‐3H (18.5 Ci‐685 GBq/mmol), 2(2,4‐dichlorophenoxy‐5‐3H)‐propionic acid (20.7 Ci‐766 GBq/mmol), 2(2,4‐dichlorophenoxy)‐propionic acid‐3‐3H (0.39 Ci‐14.4 GBq/mmol), and 4‐chlorophenoxyacetic acid‐2‐3H (13.3 Ci‐492 GBq/mmol).
Synthesis of iodobuprenorphine for use in radioimmunoassay
Authors: Debrabandere L. , van Boven M. , Daenens P. 
Published: October 2006

AbstractThe synthesis of [125I]iodobuprenorphine is described. This compound has been used as a tracer molecule in the development of a new radioimmunoassay for buprenorphine. The parameters that effect the direct iodination of buprenorphine using sodium [127I]iodide, in the presence of either chloramine‐T or Iodo‐Beads®, were previously studied. The structure of iodobuprenorphine was confirmed by mass spectrometry.
Synthesis of [14C]‐N‐[(trimethylamineboryl) carbonyl]‐phenylalanine‐methyl ester
Authors: Miller Merrill C. , Wyrick Steven D. , Hall Iris H. , Sood Anup , Spielvogel Bernard F. 
Published: October 2006

AbstractReported is the synthesis of [14C]‐L‐N‐[(trimethylamineboryl)carbonyl]‐phenylalanine methyl ester, a boron containing α‐amino acid dipeptide analog with anti‐neoplastic, anti‐inflammatory, and hypolipidemic activities. The 14C label is universally distributed among all carbon positions of the phenylalanine portion of the molecule. Briefly, the dipeptide is prepared by reacting the phenylalanine methyl ester hydrochloride salt with trimethylamine‐carboxyborane, triphenylphospine (TPP), CCl4, and triethylamine (TEA) in acetonitrile, for 24 hours. The final product afforded a specific activity of 5.71 mCi/mmol.
Synthesis of 14C‐radiolabeled ractopamine hydrochloride
Authors: Terando Norman H. 
Published: October 2006

AbstractRactopamine HCl was uniformly labeled with carbon‐14 in one of two phenyl rings as a requirement for animal metabolism studies. The six‐step synthesis was completed in a 14% yield. Product instability on silica gel complicated purification, but development of a chromatographic method afforded ractopamine ·HCl‐14C with a radiochemical purity of 98.2%.
Synthesis of 14C‐Labelled Cefclidin (E1040)
Authors: Sugiyama Isao , Woolley G. T. , Mizuo Hitoshi , Yamauchi Hiroshi 
Published: October 2006

AbstractCefclidin (E1040), a new injectable cephalosporin with potent antipseudomonal activity, was synthesized labelled with carbon‐14, starting from bromo[1‐14C]acetic acid according to the method illustrated in Scheme 1, 2. [14C] Cefclidin, having a specific activity of 3.43 MBq/mg (water content 15.3%, which was based on water content of non labelled compound prepared by the same procedure), was obtained in 2% overall radiochemical yield, with a radiochemical purity of more than 99.1%.
Synthesis of four tritium‐labelled aminowarfarin methyl ketal regioisomers
Authors: Obach R. Scott , Kaminsky Laurence S. 
Published: October 2006

Abstract6‐Bromo‐4′‐nitro‐, 4′‐bromo‐6‐nitro‐, 4′‐bromo‐7‐nitro‐ and 4′‐bromo‐8‐nitrowarfarin methyl ketals were prepared and together subjected to catalytic tritiation over palladium on charcoal to produce tritium‐labelled aminowarfarin methyl ketals. The four regioisomers were separated by thin‐layer chromatography to yield pure compounds of high (24.9–29.8 Ci/mmol) specific activity.
Synthesis of S‐[3‐(4(5)‐imidazolyl)propyl],N‐[2(4‐{125I}‐iodophenyl)ethyl]isothiourea sulfate (125I‐iodophenpropit), a new probe for histamine H3 receptor binding sites.
Authors: Menge Wiro M. P. B. , Goot Henk Van Der , Timmerman Hendrik , Eersels Jos. L. H. , Herscheid Jacobu S. D. M. 
Published: October 2006

AbstractThe synthesis of the first high specific activity {125I} labelled selective H3 antagonist, Iodophenpropit‐ i.e., S‐[3‐(4(5)‐imidazolyl)propyl],N‐[2‐(4‐{125I}‐iodophenyl)ethyl]isothiourea sulfate is reported.The radiolabelled compound was prepared by Cu(I)assisted nucleophilic non‐isotopic exchange from the corresponding bromo derivative (VUF 4598). The 125I‐Iodophenpropit was purified using reverse phase HPLC and obtained in a chemical and radiochemical purity >98% and a specific activity of 1900 Ci/mmol.
A Convenient method to synthesize specifically labelled cholesterol with tritium
Authors: Malik Sohail , Kenny Margaret , Ahmad Suhail 
Published: October 2006

AbstractA simple method is described to label cholesterol with tritium. Cholesterol was first oxidized to 5‐cholesten‐3‐one (2) which was then purified by HPLC. Its structure was established by electron impact (EI) mass spectrometry and 1H‐NMR spectroscopy. The ketone (2) was reduced with NaB3H4 to give specifically labelled cholesterol (C‐33H) at low specific activity.
A convenient method to synthesize N‐[3H]methyl‐N‐nitrosocarbamate transfer reagents
Authors: Mehta Pratibha , Konakahara Takeo , Gold Barry 
Published: October 2006

AbstractActivated N‐alkyl‐N‐nitrosocarbamates are useful acyl transfer reagents that are employed in the synthesis of N‐alkyl‐N‐nitrosoureas and related N‐nitroso compounds. The nitrosourea products are of chemical and biological interest because they provide access to the in situ generation of highly reactive carbonium type intermediates, which, depending on their structure, can be powerful carcinogens or antineoplastic agents. The availability of radiolabeled nitrosoureas greatly facilitates studies on their chemical and biological activities. Generally, the synthesis of activated nitrosocarbamates requires condensation of radiolabeled alkylisocyanates with the appopriate alcohol. Because radiolabeled alkylisocyanates are not commercially available and/or troublesome to synthesize, we have developed an easy and economical method for preparing N‐[3H]methyl‐N‐nitrosocarbamates suitable for use as transfer reagents utilizing 1,2,2,2‐tetrachloroethyl chloroformate and [3H]methylamine hydrochloride as starting materials.
Synthesis and analysis of the opioid analgesic [14C]‐fentanyl
Authors: Bagley Jerome R. , Wilhelm Jeffrey A. 
Published: October 2006

AbstractThe synthesis of [14C]‐fentanyl, the radiolabelled congener of the potent opioid analgesic chosen for utilization in drug disposition studies, is described. [14C]‐Labelling was achieved in the first of two steps, a room temperature reduction of the in situ generated Schiff base from 1‐phenylethyl‐4‐piperidone and [UL‐14C]‐aniline hydrochloride with sodium triacetoxyborohydride. A nearly instantaneous production of fentanyl was accomplished at room temperature with the addition of propionyl chloride. The overall radiochemical yield was 18%. The method described is efficiently adaptable for submicromolar scale while yielding a product of sufficient specific activity for in vivo studies. Our solvent system for thin layer chromatography was superior to the USP system reported for chromatographic analysis of fentanyl. This is the first reported preparation of [14C]‐fentanyl with the radiolabel in the aniline benzene ring.
A study of irradiation conditions of mercury target with protons to obtain thallium‐201
Authors: Fernandes Lizete , da Silva Constǎncia P. G. 
Published: October 2006

AbstractThe 201T1C1 solution is used in Nuclear Medicine for myocardial visualization. 201T1 is a cyclotron‐produced radioisotope, obtained indirectly from the decay of 201Pb or directly by irradiating mercury with protons. In this work, 201T1 was obtained by irradiating a natural mercury target with protons in the energy range of 24 to 19 MeV, using the IPEN's CV‐28 cyclotron. Range calculations of protons in the targets and in the materials used to degrade the proton beam energy were made. At the end of the bombardment of a 329 μm thickness (6 MeV thickness) target of natural metallic mercury with 19 MeV protons provided a yield of 10 MBq 201T1/μA.h.
Microbiological preparation of D‐[3,4‐13C2]glucose
Authors: Baxter Robert L. , Baxter Helen C. , McGregor Christopher J. 
Published: October 2006

AbstractA simple and effective synthesis of D‐[3,4‐13C2]Glucose (60 atom % 13C2) via 13C enriched α,α' trehalose (1) produced from sodium [1‐13C]acetate by sporulating yeast is described.
Synthesis of Hexadecylphospho[methyl‐14C]‐choline
Authors: Geilen C. C. , Samson A. , Wieder Th. , Wild H. , Reutter W. 
Published: October 2006

AbstractHexadecylphospho[methyl‐14C]‐choline was synthesized in two steps from the tetra‐n‐butyl‐ammonium salt of phosphoryl[methyl‐14C]‐choline and 1‐bromohexadecane, and purified by column chromatography on silica gel. The total yield of the radioactive synthesis was 35%, whereas the total yield of the non‐radioactive synthesis was 40%. Hexadecylphospho[methyl‐14C]‐choline may serve as a useful tool for pharmacokinetic and biochemical studies of this new antitumor drug.
An elegant synthesis of [1‐14C] hexadecyltrimethylammonium bromide [CTAB]
Authors: Gurudutt K. N. , Srinivas P. , Srinivas S. 
Published: October 2006

AbstractHexadecyltrimethylammonium bromide, a cationic detergent having a wide range of applications, was synthesised from [1‐14C] hexadecanoic acid via its methyl ester, alcohol and bromide, in an overall yield of 84%. It had a specific activity of 6.30 uCi/mmol and a radiochemical purity of 97.6%.
Synthesis of carbon‐14 labeled vigabatrin
Authors: Schuster Albert J. , Wagner Eugene R. 
Published: October 2006

AbstractCarbon‐14 labeled vigabatrin was synthesized in 5 steps from 5‐hydroxymethyl‐2‐pyrrolidone tosylate and NaCN‐[14C]. A key step involved reduction of the resulting nitrile in the presence of excess dimethylamine to give the dimethylamino‐ethyl 2‐pyrrolidone derivative in one step. This afforded an overall radiochemical yield of 22% and radiochemical purity greater than 98%.
Carbon‐11 labelling of an inhibitor of acetylcholinesterase: [11C]physostigmine
Authors: Bonnot‐Lours S. , Crouzel C. , Prenant C. , Hinnen F. 
Published: October 2006

AbstractPhysostigmine, an alkaloid from calabar bean is a strong inhibitor of acetylcholinesterase (Ki=3.33 ± 0.26 × 10−6M) and has been used clinically in the treatment of glaucoma, atropine intoxication, myasthenia gravis and more recently, in experimental trials in Alzheimer's disease. In order to study the AChE activity in the brain by positron emission tomography, we have undertaken the labelling of physostigmine with carbon‐11. The synthesis involves the reaction of [11C]methylisocyanate with eseroline. [11C]Methylisocyanate was obtained by heating [11C]acetylchloride with tetrabutylammonium azide in toluene. The synthesis of [11C]CH3COCl involves the carbonation of methylmagnesium bromide in THF with cyclotron produced [11C]carbon dioxide and the addition of phthaloyl dichloride. The [11C]methylisocyanate is distilled into a solution of eseroline in ether with a small piece of sodium. After 10 minutes at 25°C, the solution is purified by HPLC and the appropriate fraction collected.Starting with 55.5 GBq (1.5 Ci) of [11C]carbon dioxide, 0.92‐1.48 GBq (25‐40 mCi) of [11C]Physostigmine are obtained 57 minutes after EOB.
Synthesis of a novel 123I‐labelled derivative of GBR12783, a potential agent for SPECT imaging of dopamine‐reuptake sites
Authors: He Xiao‐Shu , Lee Kan Sam , Weinberger Daniel , de Costa Brian R. 
Published: October 2006

Abstract[123I]1‐[2‐(Diphenylmethoxy)ethyl]‐4‐[3‐(m‐iodophenyl)‐2‐propenyl]piperazine ([123I]2), a potential SPECT imaging agent for dopamine reuptake sites was efficiently synthesized in 4 steps from 1‐[2‐(diphenylmethoxy)ethyl]piperazine (3). A key step in the synthesis was the selective AIH3‐mediated reduction of 1[2‐(diphenylmethoxy)ethyl‐4‐(m‐bromocinnamoyl] piperazine (4) to 1‐[2‐(diphenylmethoxy)ethyl‐4‐(3‐(m‐bromophenyl)‐2‐propenyl]piperazine(5). The 123I label of [123I]2 was introduced in the final step in up to 90% radiochemical yield by treatment of the organotin precursor 1‐(2‐(diphenylmethoxy)ethyl‐4‐[3‐[(m‐(tributyl stannyl)phenyl]‐2‐propenyl]piperazine (6) with Na123I in aqueous CH3CO3H.
A convenient method for the synthesis of radioactively labelled aryl glycosides
Authors: Griffin Simon D. J. , Donaldson Iain A. 
Published: October 2006

AbstractFluoride‐directed methylation of the aryl hydroxyl of hydroxyphenyl glycosides with radioactive methyl iodide allows the incorporation of label under mild conditions that preserve the glycosidic link. The effectiveness of this approach has been demonstrated by the synthesis of two 14C‐labelled aryl α‐glycosides.
A comparison of the incorporation of 123I and 18F into 1‐[1‐(3‐hydroxyphenyl) cyclohexyl]‐4‐(methanesulfonyloxy)piperidine by nucleophilic displacement with 123I− and 18F−
Authors: He Xiao‐Shu , Kiesewetter Dale O. , Lee Kan Sam , Mattson Mariena V. , Weinberger D. R. , de Costa Brian R. 
Published: October 2006

AbstractUnlabelled and labelled 4‐fluoro‐ and 4‐iodo‐1‐[1‐(3‐hydroxyphenyl)cyclohexyl]piperidines (3 and 4, respectively), derivatives of phencyclidine, were synthesized in 3‐steps via nucleophilic displacement reaction of 1‐[1‐(3‐hydroxyphenyl) cyclohexyl]‐4‐(methanesulfonyloxy)piperidine (8). The displacement reaction with 3 molar equivalents of Bu4N+I− gave 58% of 4 with no detectable methanesulfonate elimination. Reaction of a large excess of 8 with Na123I− under similar conditions gave up to 40% yield of [123I]8. In contrast reaction of 8 with 3 molar equivalents of unlabelled Bu4N+F− in refluxing acetonitrile yielded only 3.1% of 3 and 97% of elimination product. Similarly, reaction of a large excess of 8 with Bu4N+18F− at 80 °C in acetonitrile failed to yield detectable quantities of [18F]3. However, low (0‐4%) yields of [18F]3 were obtained using 18F− in the presence of varying proportions of inorganic base and Krytofix in acetonitrile.
A one‐pot synthesis of (±)‐(ring 13C6)‐mandelic acid
Authors: Sirimanne Sarath R. , Patterson Donald G. 
Published: October 2006

AbstractA one‐pot synthesis of (±)‐(ring 13C6)‐mandelic acid is reported. [Ring 13C6]‐benzaldehyde was cyanosilylated with trimethylsilyl cyanide (TMSCN)/Znl2. The resulting cyanosilylated adduct was hydrolyzed with concentrated hydrochloric acid without purification. The workup involves evaporation to dryness and extraction of the (±)‐(ring 13C6)‐mandelic acid with hot benzene. After one crystallization, the synthesis produced an overall yield of 65% of (±)‐(ring 13C6)‐mandelic acid that was about 98% pure by HPLC with UV detection.
Racemic synthesis and enantiomeric conversion of [1‐13C] valine
Authors: Polach Kevin J. , Shah Sapan A. , Laiuppa John C. , Lemaster David M. 
Published: October 2006

AbstractA Strecker synthesis of isobutyraldehyde, K13CN and ammonia produced D,L‐[1‐13C] valine in 83% yield. This racemic mixtue was then converted to the L‐form via a D‐amino acid oxidase ‐ branched amino acid aminotransferase system in an overall yield of 75% based on K13CN. Given the generality of the Strecker synthesis as well as the broad substrate specificity of the oxidase and aminotransferase enzymes, it is anticipated that this procedure will be comparably efficient for most standard aliphatic and aromatic amino acids.
The preparation of tritium labelled biocompatible polymers
Authors: Russell Jeremy C. , Jones John R. , Vick Terrence A. , Stratford Peter W. 
Published: October 2006

AbstractThe preparation of tritiated phosphoryl choline containing linear polymers by the reduction of an acetylenically unsaturated polymer with tritium gas is described. Homogeneous catalysis was used and the product was analysed by 1H and 3H‐nmr spectroscopy. The use of lanthanide shift reagents showed that 98% of the isotope was located in the 7 and 8 positions of the hydrophobic chains.
Synthesis of 11‐[3H]‐arteether, an experimental antimalarial drug
Authors: Pu Yu‐Ming , Ziffer Herman 
Published: October 2006

AbstractThe triphenylphosphine hydrobromide‐catalyzed addition of a proton from ethanol to anhydrodihydroartemisinin (5) has been employed for the synthesis of 2 and 4 Use of 1.5 equivalents of EtO2H or EtO3H yielded 11‐[3H]‐β‐arteether as the major product.
Synthesis of the enantiomers and three racemic metabolites of carvedilol labeled to high specific activity with tritium
Authors: Senderoff S. G. , Villani A. J. , Landvatter S. W. , Garnes K. T. , Heys J. R. 
Published: October 2006

AbstractCarvedilol (SK&F 105517) possesses unique cardiovascular activity, and is under development for indications such as angina and hypertension. Tritium labeled enantiomers of Carvedilol and racemates of three metabolites were needed for pharmacologic and drug metabolic studies. These compounds were synthesized by catalytic tritium‐halogen exchange using tritium gas and 10% palladium‐on‐carbon catalyst. The precursors were polyhalogenated in the carbazole ring. Direct electrophilic bromination of the enantiomers of Carvedilol gave precursors that were converted to the corresponding tritiated final products by catalytic tritium halogen exchange. Bromination of 4‐(2,3‐epoxypropyloxy)‐9H‐carbazole gave an intermediate that was converted to the halogenated precursors of the racemic metabolites. Elaboration of this intermediate, 1,3,6‐tribromo‐4‐(2,3‐epoxypropyloxy)‐9H‐carbazole, to the desired metabolite precursors was achieved by nucleophilic epoxide opening with suitably functionalized N‐benzyl aryloxyethylamines. Catalytic tritium‐halogen exchange upon the brominated metabolite precursors was accompanied by cleavage of N‐ and Q‐benzyl protecting groups. Radiochemical purities of all tritiated final products were greater than 98% after preparative HPLC. Specific activities of the final products, determined by mass spectrometry, ranged from 35 to 76 Ci/mmol. Optical purity of the Carvedilol enantiomers, determined by chiral HPLC, was greater than 99%
A facile synthesis of sodium 3‐[1‐14C]‐ethyl‐7‐isopropyl‐1‐azulenesulfonate
Authors: Shimada Takeshi , Yanagisawa Takashi , Tomiyama Tsuyoshi , Okazaki Mitsuo 
Published: October 2006

AbstractSodium 3‐ethyl‐7‐isopropyl‐1‐azulenesulfonate1, a new therapeutic agent for stomatitis, pharyngitis and ophthalmia was labelled with carbon‐14 in the ethyl group attached to the azulene ring for use in metabolic studies.14C‐labelled1with a specific activity of 1.98 GBq/mmol was prepared in four steps in 39.3% overall chemical yield from [1 ‐14C]acetic acid sodium salt.
Synthesis of [32P]labelled 1‐O‐alkyl‐2‐desoxy‐2‐amino‐sn′‐glycero‐3‐phosphocholines
Authors: Deigner H. P. , Fyrnys B. 
Published: October 2006

AbstractThe syntheses of N‐substituted 1‐O‐alkyl‐2‐desoxy‐2‐amino‐sn‐glycero‐3‐[32P]phosphocholines were performed in four steps starting from [32P] POCl3 and the corresponding 1‐O‐alkyl‐2‐amino‐propane‐3‐ols in 5‐7% total yield.
Synthesis of [methyl‐14C]‐N‐methylputrescine
Authors: Secor H. V. , Izac R. R. , Hassam S. B. , Frisch A. F. 
Published: October 2006

Abstract[Methyl‐14C]‐N‐methylputrescine was prepared from [14C]methylamine hydrochloride in five steps. Reaction of benzaldehyde and [14C]methylamine (10 mCi) followed by catalytic hydrogenation yielded [methyl‐14C]‐N‐methylbenzylamine. The key step in this process is the alkylation of [methyl‐14C]‐N‐methylbenzylamine in aqueous medium with 4‐bromobutyronitrile. The radiochemical purity of the final product after two successive catalytic hydrogenations was in excess of 97%. The radiochemical yields in two successive runs were 26 and 38%, based on starting [14C]methylamine, with specific activities of 22 and 23 mCi/mmol, respectively. This sequence provides a convenient and efficient regioselective radiosynthesis of [methyl‐14C]‐N‐methylputrescine.