bluuebunny/crossref_metadata_2025_split huggingface dataset:
Stable isotope labeled alpha‐ketoacids
Authors: Yuan Sun‐Shine , Ajami Alfred M. 
Published: October 2006

AbstractAlkylation of diethyl oxalpropionate with [D3]methyl iodide followed by acid hydrolysis led to 3‐[D3]methyl‐2‐oxobutyric (α‐ketoisovaleric) acid. Alkylation of N‐t‐butylpropylimine with [D3]methyl iodide followed by hydrolysis gave 2‐[D3]methylpropanal. This was further alkylated with 2,2‐difluoro‐1‐tosyloxyvinyllithium and hydrolyzed to afford 4‐[D3]methyl‐2‐oxopentanoic (α‐ketoisocaproic) acid. Diazotization of [1‐13C]leucine ethyl ester with t‐butylnitrite followed by peracid oxidation and hydrolysis gave [1‐13C]4‐methyl‐2‐oxopentanoic acid. In each case, the α‐ketoacids were isolated as sodium salts.
A convenient preparation of 14C‐labelled 5H‐2,3‐benzodiazepines
Authors: Zólyomi G. , Láng T. , Körösi J. , Hámori T. 
Published: October 2006

AbstractA convenient method for preparing 5H‐2,3‐benzodi‐azepines labelled with 14C was developed in which the corresponding phenylacetone derivatives were acylated by labelled aromatic carboxylic acid. In spite of the low yield, this method is advantageous in comparison the known ones because of the obtainable specific activity, which is a consequence of the few stages and simplicity of the synthesis.
Synthesis of [3H] porfiromycin
Authors: Swigor J. E. , Pittman K. A. 
Published: October 2006

AbstractThe synthesis of the title compound (1) is described. The reaction of a specific amount of [3H] methyl iodide under controlled conditions with naturally occurring mitomycin C produced [3H] porfiromycin with an overall yield of 61% and a radiochemical purity of 98%.
The synthesis of α‐methylstyrenes with 14C‐labelling in the side chain
Authors: Ali H. M. , Barson C. A. , Coe P. L. 
Published: October 2006

Abstractα‐Methylstyrenes with all three side chain carbons specifically 14C‐labelled have been synthesised by Wittig reactions between the appropriately labelled acetophenones or methylene triphenylphosphoranes. The yields in all cases were good and any radiochemical impurities could be readily removed by distillation.
Synthesis of hydroxyl[13N]amine and binding of 13NH2OH to two transaminases
Authors: Kaseman Deborah S. , Cooper Arthur J. L. , Meister Alton , Gelbard Alan S. , Reiman Robert E. 
Published: October 2006

AbstractNH2OH was labeled with a β+emitter (13N, t1/2 = 9 96 min.). Hydroxyl[13N]amine was synthesized from HSO and [13N]nitrite (produced via the 160(p,α)13N reaction by proton bombardment of H2O). The synthesis reactions are: magnified image Hydroxyl[13N]amine was purified by ion‐exchange chromatography on Dowex‐1 × 8 (AcO−) to remove unreacted 13NO and 13NO. Radiochemical yields of 50–90% were obtained in 25–30 min. The purity and specific activity of 13NH2 OH were determined by HPLC analysis and spectrophotometric assay. The binding of 13NH2 OH to pig heart glutamate‐pyruvate transaminase and to pig heart glutamate‐oxaloacetate transaminase was measured. This work demonstrates that quantitation of the binding of hydroxylamine (an active‐site directed enzyme inhibitor) labeled with a positron‐emitting isotope is technically feasible.
Preparation of [131I] iodinated nonoxynol‐9
Authors: Agha Bushra J. , Garbolas George A. , Wets Kathleen , Digenis George A. 
Published: October 2006

AbstractA novel method for the radioiodination [131I] of the multicomponent non‐ionic surfactant nonoxynol‐9 (N‐9) is described. The extent of incorporation and distribution of the 131I‐label into the aromatic moiety of various ethoxymer units of N‐9 was determined utilizing a high pressure liquid chromatographic (HPLC) method.
Fast low temperature ultrasonic synthesis and injection ready preparation of carrier free 17‐I‐123‐heptadecanoic acid
Authors: Mertens John , Vanryckeghem Wim , Bossuyt Axel , Van Den Winkel Pierre , Vandendriessche René 
Published: October 2006

Abstract17‐I‐123‐heptadecanoic acid is prepared carrier‐free from 17‐Br‐heptadecanoic acid in methyl ethyl ketone at 100°C. A quantitative labeling yield is obtained within 20 minutes using a 50 KHz ultrasonic bath. Sonication allows the presence of water up to 7.5% v/v. The pattern shown by the plot of the kinetic curves is typical of two consecutive reactions: the first being the dissociation of a radioactive side product, the second a I− for Br nucleophilic exchange. The pure carrier‐free radioiodinated fatty acid is obtained by HPLC separation and is used clinically in a sterile 6% human serum albumine solution. The quality control of the injection ready solution is based on the use of a RP18 Sep‐PakR cartridge.
Reduction of iminium ethers with sodium boro[3H] hydride. Preparation of tritium labelled clomiphene and nitromiphene (CI 628)
Authors: Ruenitz Peter C. , Bagley Jerome R. 
Published: October 2006

AbstractThe preparation of [3H]‐clomiphene and [3H]‐nitromiphene from amido precursors in a two‐step reaction sequence utilizing NaB H4 is described. The radiochemical yield and specific activity of the former are 34% and 16 mCi/mmol and those of the latter were 42% and 20 mCi/mmol, respectively. The method described is of micromolar scale designed for maintaining cost economy in the purchase of expensive radiolabelled reagents while yielding final products of sufficient radioactivity for in vitro and in vivo metabolism studies.
Synthesis of [14C]2‐pipecolinyl‐5‐amino‐4′‐chloro‐benzophenone (LF.1695)
Authors: Luu‐Duc C. , Béney C. , Le Bars D. , Charlon C. , Marsura A. , Bellamy F. , Ou K. 
Published: October 2006

AbstractTwo synthetic routes lead to [14C] LF.1695. The first one starts with labelled triphenyl methyl phosphonium iodide. This Wittig reagent reacts with benzyl piperidinone to afford benzylmethylidene piperidine 3. The reduction of 3 gives labelled pipecoline 4 which is condensed with an adduct affording an intermediate nitro compound 5. LF.1695 6 labelled at the methyl group is then obtained by catalytic reduction.The second route uses labelled chloro‐nitro benzoic acid as starting material. The treatment of the corresponding acid chloride by Friedel‐Crafts reaction gives the chloro‐nitro‐chloro‐benzophenone 9 in good yield. Condensation of 9 with pipecoline according to the method described above gives an intermediate nitro compound 10 which is reduced to afford LF.1695 11 labelled at the carbonyl group.
Regioselective synthesis of unsymmetrical deuterium labelled hydrazines and azoxy compounds
Authors: Cooper Curt S. , Weinkam Robert J. 
Published: October 2006

AbstractA method for the preparation of deuterium labelled unsymmetrical hydrazines was developed. This method was used to prepare l‐benzyl‐2‐methyl‐2H3‐hydrazine hydrobromide and l‐benzyl‐2H7‐2‐methylhydrazine hydrobromide, analogs of the cancer chemotheraputic agent procarbazine. These compounds were then used to prepare the corresponding labelled benzyl‐(ONN) and (NNO)‐azoxymethane isomers. A method was developed whereby the deuterium labelled azoxy isomers were separated by reversed phase semi‐preparative HPLC.
Synthesis of 4‐(2‐chlorophenyl)‐1, 6‐dihydro‐1, 3, 9‐trimethylimidazo[1, 2‐a]pyrazolo[4, 3‐f] [1, 4]diazepine‐9‐14C (CI‐918‐14C)
Authors: Hicks James L. , Huang C. C. , Goel Om P. , Butler Donald E. 
Published: October 2006

Abstract4‐(2‐Chlorophenyl)‐1, 6‐dihydro‐1,3,9‐trimethylimidazo[1,2‐a]pyrazolo‐[4,3‐f] [1,4]diazepine‐9‐14C (CI‐918‐14C) was made starting with acetyl‐1‐14C chloride. An efficient synthesis of 1‐chloro‐2‐propanone‐2‐14C was developed as a precursor to 2‐methyl‐1,3‐dioxolane‐2‐14C‐2‐methanamine. The latter reacted with 4‐(2‐chlorophenyl)‐1,6‐dihydro‐1,3‐dimethylpyrazolo[3,4‐e] [1,4]diazepine‐7‐thione to yield 4‐(2‐chlorophenyl)‐1,6‐dihydro‐1, 3‐dimethyl‐N‐[(2‐methyl‐1,3‐dioxolan‐2‐yl‐2‐14C)methyl] pyrazolo[3,4‐e] [1,4]diazepin‐7‐amine. Hydrolysis and cyclization gave the title compound. The six‐step reaction sequence gave an overall radiochemical yield of 19%. The product had a specific activity of 8.31 mCi/mmol.
Synthesis of 14C‐anthralin
Authors: Brown C. , Eustache J. , Frideling J. P. , Shroot B. 
Published: October 2006

Abstract1,8‐dihydroxy‐[10‐14C]9‐anthrone (anthralin) was synthesized in good yield starting from readily available 3‐methoxy‐2‐(2‐methoxybenzyl)‐benzoic acid (3).14C was introduced via carboxylation of the Grignard derived from 3‐bromo‐2(2‐methoxybenzyl) anisole. This, in turn, was obtained from (3) by a Curtius and Sandmeyer reaction sequence.
Synthesis of N‐[2‐3H] acetyl‐D‐muramyl‐L‐alanyl‐D‐iso‐glutaminyl‐L‐alanyl‐2‐(1′,2′‐dipalmitoyl ‐sn‐glycero‐3′‐phosphoryl) ethylamide of high specific radioactivity
Authors: Brundish D. E. , Wade R. 
Published: October 2006

AbstractThe title compound (MTP‐cephalin) was synthesised with specific activity of 22 Ci mmol−1 and with radiochemical purity of 96–98% by a direct radiochemical synthesis using [3H] muramyl dipeptide. Several unsuccessful approaches to the target compound are documented.
Radiolabelling of the histamine liberating sesquiterpene lactone, thapsigargin
Authors: Br Christensen S. ØGger 
Published: October 2006

AbstractThapsigargin (1) selectively labelled in the butyrate moiety of the molecule was isolated after hydridocarbonyltris (triphenylphosphine) rhodium (I) catalyzed reduction of the product (5) obtained by reacting debutanoylthapsigargin (2) with 3‐butenoic anhydride. The use of tritium gas as a reducing agent afforded labelled thapsigargin with a specific activity of 78 Ci/mmol.
Synthese DU cyclopropylmethyl‐2 di(paramethoxyphenyl)‐5,6 oxo‐3 triazine‐1,2,4 (14C‐3) (ST 1118)
Authors: Bonnaud B. , Cousse H. , Noël J. P. , Pichat L. , Pitet G. 
Published: October 2006

Abstract(14C) semicarbazide hydrochloride was obtained from (14C) urea and hydrazine hydrate. It was condensed with 1,2‐di‐ (4‐methoxy phenyl)‐ethane‐1,2‐dione giving rise to 5, 6‐di‐(4‐methoxyphenyl)‐3‐oxo‐(3‐14C)‐1,2,4‐triazine. The latter, after condensation with bromomethyl cyclopropane gave (3‐14C) ST 1118 : 2‐(cyclopropylmethyl)‐5,6‐di‐(4‐methoxyphenyl)‐3‐oxo‐(3‐14C)‐1,2,4‐ triazine. The overall yield based on urea was 37.2%. After silicagel column chromatography and crystallisation the radiochemical purity was 99.5% ‐ Specific activity : 5.8 mCi/mMole.
Synthesis of pyrilamine‐d6
Authors: Bird Ian , Shuker David E G 
Published: October 2006

AbstractPyrilamine‐d6 (N‐[(4‐methoxyphenyl)methyl]‐N′, N′‐di[2H3]methyl‐N‐2‐pyridinyl‐1,2‐ethanediamine) was synthesised from N‐2‐[(4‐methoxyphenyl)methyl]‐aminopyridine and 2‐(N,N‐di[2H3]methylamino)ethyl chloride in 83% yield. The alkyl chloride was prepared in 37% overall yield in a three step reaction from toluene‐4‐sulphondi [2H3]methylamide.
Convenient preparation of deuterated uracils and dihydrouracils
Authors: Hill Richard K. , Ledford N. Dale , Renbaum Louis A. 
Published: October 2006

AbstractThe reaction of [3‐2H1]propiolic acid with urea provides a simple route to [6‐2H1]uracil, and further exchange with DCl affords [5,6‐2H2]uracil. Reaction of the meso and d, 1‐isomers of [2,3‐2H2]succinamide with lead tetraacetate leads to the cis and trans isomers of [5,6‐2H2]5,6‐dihydrouracil.
Synthesis and unusual NMR spectra of 4,4′‐dinitro‐3,3′‐bifurazanyl‐4,4′‐13C
Authors: Coburn Michael D. 
Published: October 2006

AbstractThe synthesis of 4,4′‐dinitro‐3,3′‐bifurazanvl‐4,4′‐13C was accomplished starting with sodium cyanide‐13C and dichloroglyoxime. The carbon‐13 NMR spectrum of the product consists of a 1,1, l‐triplet and the nitrogen‐14 NMR spectrum contains a sharp doublet with the same coupling constant as the carbon‐13 triplet.
Tritium labelled (±)‐7‐chloro‐8‐hydroxy‐3‐methyl‐1‐phenyl‐2,3,4,5‐tetrahydro‐1H‐3‐benzazepine (SCH23390)
Authors: Wyrick Steven D. , Mailman Richard B. 
Published: October 2006

AbstractThe antipsychotic drug, SCH23390, once thought to be the first selective D1 dopamine antagonist, is now believed to possibly produce its profound antidopaminergic and antipsychotic effects via molecular sites that involve recognition characteristics similar to, or are a subpopulation of the D1 dopamine receptors. Tritium labelled SCH23390 has been prepared in our laboratory by palladium catalyezed reductive aryl debromination of a brominated precursor with carrier free tritium gas in THF. The product is labelled in the 9‐position of the benzazepine ring and a specific activity of 5.6 Ci/mmole was obtained.
Synthesis of 14C‐labelled milrinone
Authors: Duncan D. R. , Johnston D. , Andrews R. S. 
Published: October 2006

AbstractA synthetic procedure for producing 14C‐labelled milrinone is described. The synthesis was achieved in two steps from 1‐(4‐pyridyl)propan‐2‐one utilising [2‐14C]cyanoacetamide as the source of the radiolabel. The overall chemical yield was 46% and the radiochemical yield 35%.
Synthesis of carbon‐14 labeled clomiphene
Authors: Rao P. Narasimha , Cessac James W. 
Published: October 2006

AbstractClomiphene, 2‐[4‐(2‐chloro‐1,2‐diphenylethenyl)phenoxy]‐N, N‐diethylethanamine, an antiestrogen, is a nonsteroidal triphenylethylene derivative. For the successful synthesis of carbon‐14 labeled clomiphene it is essential to have a free radical inhibitor in the reaction medium.
Preparation and purification of 125I‐labeled iodospiroperidol
Authors: Landvatter Scott W. 
Published: October 2006

AbstractIodine‐125 labeled spiroperidol has been synthesized by a simple, one‐step procedure starting from spiroperidol. This synthesis employs 125I‐ and H2O2 in buffered acetic acid. This pH dependent reaction affords iodospiroperidol in 40% radiochemical yield and a specific activity, after HPLC purification, of ca. 1900 Ci/mmol.
Synthesis of iodine‐125 labelled ω‐iodoundecyl cholesteryl ether
Authors: Kabalka George W. , Varma Rajender S. , Jinaraj Vadeparambil K. , Huang Leaf , Painter Susan K. 
Published: October 2006

Abstractω‐[125I]Iodoundecyl cholesteryl ether has been synthesized via a hydroboration‐iodination sequence. The syntheses can be used to prepare high specific activity (no‐carrier‐added) reagents.
Synthesis, 1H‐NMR and mass spectra of 2‐2H‐, 2,3‐2H2‐ and 2,2‐2H2‐labelled short chain carboxylic acids
Authors: Hine David G. , Ikeda Yasuyuki , Tanaka Kay 
Published: October 2006

Abstract2‐2H, 2,3‐2H2 and 2,2‐2H2 ‐ short chain carboxylic acids were synthesized. Monodeuteration at the 2‐position of the carboxylic acids was achieved via decarboxylation of the corresponding carboxyldeuterated 2‐alkylmalonic acids. 2,3‐Dideuteration was achieved via catalytic deuteration of the corresponding 2,3‐ unsaturated carboxylic acids with sodium borodeuteride. 2,2‐Dideuteration was achieved via repeated base catalyzed exchange reactions of the carboxylate sodium salts in sodium deuteroxide/deuterium oxide solution. Proton nuclear magnetic resonance and mass spectra of the obtained products are presented.
Synthesis of (21‐3H3)‐pregnenolone
Authors: Prasad V. V. Kris , Franklin Steven O. 
Published: October 2006

AbstractA simple procedure for the preparation of 21‐3H ‐ pregnenolone using pregnenolone as starting material is described. The procedure involved removal of the C‐21‐methyl group of the steroid and the side‐chain was reconstructed with 3H CH3MgI in two steps: a Grignard reaction followed by oxidation of the resulting alcohol. An overall yield of 71% was achieved.
75,77Br‐Nor‐zimelidine: Radiohalogenation of a complex molecule via a trimethylstannyl precursor
Authors: Kloster Gerd , Laufer Peter , Hanuš Jan 
Published: October 2006

AbstractThis communication describes the preparation of radiobrominated nor‐zimelidine (III), a potential tracer for the serotonin reuptake system of the brain, by a bromodemetallation reaction using a suitable trimethylstannyl precursor (II). (II) was prepared from NaSn (CH3)3 and nor‐zimelidine in low yield and thoroughly purified by preparative hplc. Bromodemetallation reaction using an equimolar amount of Br2 showed quantitative formation of nor‐zimelidine without any detectable side‐products. Radiobromination yields using n.c.a. 75,77Br at the 100 μCi level were 60 % with one hour preparation time including purification. Conditions were not optimized for large scale production of high specific activity (III) since the compound was withdrawn from the market by the producer during the course of this study.
Synthesis of 4‐fluoro‐4′‐trifluoromethylbenzophenone guanylhydrazone hydrochloride labeled with 14C
Authors: Wang Theodore S. T. , Fawwaz Rashid A. 
Published: October 2006

AbstractFour steps were required to synthesize the title compound. This involved carboxylation, acid chloride formation, condensation, and hydrazone formation. The overall radiochemical yield was 12.5% amd the specific activity was 2.04 mCi/mmole. Because of the difficulty encountered in preparing the p‐fluorobenzal‐dehyde‐aldehyde‐14C, p‐fluorobenzoyl chloride‐carbonyl14C was used for the condensation reaction.
Synthesis of (β‐methyl3H‐6β‐iodopenicillanic acid
Authors: De Meester Fabien , Frère Jean‐Marie , Piette Jean‐Louis , Vanderhaeghe Hubert 
Published: October 2006

AbstractA rapid and easy synthesis of tritium‐labelled β‐iodopenicillanate, an efficient inactivator of serine β‐lactamase, is described. This method involves only three reaction steps after the introduction of the label in the molecule with an overall yield of 16 %.
Radiobromination of the 1‐position of estradiol using no‐carrier‐added bromine‐77
Authors: Hylrides Mark D. , Buksa Patricia L. , Mettler Fred A. , Wilbur D. Scott 
Published: October 2006

AbstractThe target compound, 1‐([77Br]bromo)estradiol (1a), was prepared in three steps from 4‐aminoestradiol, 3‐methyl ether (2). Electrophilic bromination of 2 with in situ generated 77BrCl followed by deamination in the same reaction mixture gave 1‐([77Br]bromo)estradiol 3‐methyl ether (4a) in 59% radiochemical efficiency. Subsequent demethylation of 4a gave la in 92% radiochemical efficiency with an estimated specific activity of 300–600 Ci/mmol. An overall radiochemical yield of approximately 20% was obtained. Stability studies of la showed no decomposition over a three‐day period.
Synthesis of |24‐14C|‐23‐norcholanoic acid derivatives
Authors: Maier M. S. , Seldes A. M. , Gros E. G. 
Published: October 2006

AbstractSyntheses of |24‐14C| 3β, 20ξ‐dihydroxy‐23‐norchol‐5‐enoic acid, |24‐14C| 3β, 20ξ‐dihydroxy‐23‐norcholanoic acid and |24‐14C| 20ξ‐hydroxy‐3‐oxo‐23‐norchol‐4‐enoic acid were accomplished by reaction of ethyl |1‐14C| bromoacetate, in Reformatsky conditions, with suitable 20‐keto‐pregnane derivatives. Dehydration of these products afforded |24‐14C| 3β‐hydroxy‐23‐norchola‐5, 20(22)E‐enoic acid and |24‐14C| 3‐oxo‐23‐norchola‐4, 20(22)E‐dienoic acid respectively. The products were characterized by spectroscopic (IR, 1H NMR, MS) methods.
13C‐Labelled benzo[a]pyrene and derivatives. An efficient pathway of labelling the 1‐, 2‐, and 3‐positions
Authors: Bodine Richard S. , Daub Guido H. , Vanderjagt David 
Published: October 2006

AbstractA ten step synthesis of benzo [a]pyrene‐1‐13C, ‐2‐13C, or 3‐13C from 2,3,7,11b‐tetrahydrobenz[d, e] anthracen‐3(1h)‐one is described in which the initial step involves the condensation of this ketone with the lithium enolate of ethyl acetate. This completes our synthesis of the tweleve 13C labelled benzo[a]pyrenes.
Synthesis of [13N]cisplatin
Authors: Haber Martin T. , Cooper Arthur J. L. , Rosenspire Karen C. , Ginos James Z. , Rottenberg David A. 
Published: October 2006

AbstractA method for the “carrier‐added” synthesis of [13N]cisplatin is described. Yields were ∼1–4 mCi from 20–40 mCi of [13N]ammonia with a total synthesis time of 19–28 minutes. The product was ∼96% radiochemically pure as judged by HPLC analysis and had a specific activity of ∼100 mCi/mmole in 1.0 ml of saline. [13N]Cisplatin was administered intraperitoneally to mice. Of the tissues investigated, concentration of label was highest in kidneys. At 10 min, considerable label in the blood, liver, and kidney was in a form other than cisplatin. However, no evidence was obtained that [13N]ammonia was released from [13N]cisplatin in vivo. [13N]Cisplatin may be used to assess drug delivery to primary and metastatic brain tumors in patients receiving intravenous or intraarterial cisplatin chemotherapy.
Preparation of 2‐chloro‐6‐(2‐furanylmethoxy)‐4‐trichloromethylpyridine‐2,6‐14C
Authors: McKendry L. H. 
Published: October 2006

AbstractA 16.7 mCi sample of 99+% radiochemically pure 2‐chloro‐6‐(2‐furanylmethoxy)‐4‐trichloromethylpyridine‐2,6‐14C with a specific activity of 13.2 mCi/mmole was prepared from trimethyl citrate‐1,5‐14C in a 44% yield via a three‐step process.
Synthesis of 1‐amino‐2‐β‐(3‐ [2,6‐14C] piperidinome thylphenoxy) propylamino ‐1‐cyclobutene‐3,4‐dione hydrochloride
Authors: Swigor J. E. , Algieri A. A. , Standridge R. T. , Pittman K. A. 
Published: October 2006

AbstractThe synthesis of the title compound (6) is described. The condensation of 3‐aminopropanol with phthalic anhydride and subsequent treatment with phosphorous tribromide produced N‐[3‐bromopropyl] phthalimide. Acylation with 3‐hydroxybenzaldehyde, reduction with hydrogen over Raney nickel and subsequent treatment with thionyl chloride gave N‐[ 3‐(3‐chloromethylphenoxy) propyl ] phthalimide (2). Treatment with [2, 6 ‐ 14C] piperidine introduced the radiolabel (3). Deprotection of the amino group with hydrazine and treatment with 3‐methoxy‐4‐amino‐3‐cyclobutene‐1,2‐dione produced 1‐amino‐2‐ [3‐(3‐[ 2,6‐ 14C] piperidinome thylphenoxy) propylamino ]‐1‐cyclobutene‐3, 4‐dione (5). Treatment with hydrochloric acid yielded the title compound (6) in an overall chemical yield of 22%.
Synthesis of labelled ecdysone precursors: Part I‐tritium labelled (3H4‐22, 23,24,25)‐3β, 14α‐dihydroxy‐5β‐cholest‐7‐en‐6‐one
Authors: Haag T. , Hetru C. , Nakatani Y. , Luu B. , Pichat L. , Audinot M. , Meister M. 
Published: October 2006

AbstractHigh specific activity tritiated 3β, 14α ‐dihydroxy‐5β‐cholest‐7‐en‐6‐one, has been prepared using a precursor which permits rapid and easy labelling. This compound is converted to ecdysone under in vitro conditions by insect prothoracic glands, a well known site of ecdysone biosynthesis.
[11C]Labeling of coenzyme Q10 and its tissue distribution
Authors: Takahashi T. , Ido T. , Iwata R. , Ishiwata K. , Hamamura K. , Kogure K. 
Published: October 2006

Abstract[11C]Coenzyme Q10 was synthesized by O‐methylation of 3‐demethyl coenzyme Q10 with 11CH3I. We have produced 1–4 mCi of [11C]coenzyme Q10 with radiochemical yields of 6–16 % (based on trapping 11CH3I) in 35–50 min with radiochemical purities of >95%. The specific activity was 4–5 mCi/μMol at the end of [11C]‐coenzyme Q10 synthesis. The tissue distribution was investigated on mongolian gerbils after intravenous administration of [11C]‐coenzyme Q10 solubilized with polyoxyethylene hydrogenated caster oil (HCO‐60). The blood level of [11C]coenzyme Q10 was very high and its clearance was slow. The accumulations in the heart, kidney and liver were moderate and the accumulation in the brain was low in spite of its high lipophilicity.
Synthesis of [4′‐13C] pyridoxol
Authors: Velde V. W. Vande , Mackenzie N. E. , Scott A. I. 
Published: October 2006

Abstract5‐Cyano‐3‐hydroxy‐2‐methylpyridine‐l‐oxide, after O‐methylation with dimethylsulfate, was reacted regiospecifically with sodium [13C] cyanide to give [4′‐13C] 4,5‐dicyano‐3‐hydroxy‐2‐methylpyridine. The latter compound was successively transformed to [4′‐13C] pyridoxol and [4′‐13C] pyridoxal phosphate.
Synthesis of [1‐14C‐carboxy]‐4‐benzoylbenzoic acid
Authors: Nakamaye Kay L. , Yount Ralph G. 
Published: October 2006

Abstract[1‐14C‐Carboxy]‐4‐benzoylbenzoic acid has been prepared via a Grignard reaction with 14CO2. 4‐Bromobenzophenone was converted to (4‐bromophenyl)‐phenyldichloromethane using phosphorus pentachloride. The dichloro compound was reacted with methoxide ion to form 4‐bromobenzophenone dimethylketal which was subsequently converted to its Grignard reagent, carboxylated with 14CO2, and acid hydrolyzed to the final product. Using excess Grignard reagent, virtually quantitative conversion of 14CO2 to product was obtained.