bluuebunny/crossref_metadata_2025_split huggingface dataset:
Preparative isolation of [U‐14C]solanesol from 14CO2‐chamber grown tobacco
Authors: Hassam Saifunnissa B. 
Published: October 2006

AbstractA method for the preparative isolation of [U‐14C]solanesol from 14CO2‐chamber grown tobacco is described. Freeze‐dried tobacco leaves were Soxhlet extracted with methylene chloride. Fractionation of the extract by silica gel chromatography yielded crude solanesol. Subsequent purification by normal phase high pressure liquid chromatography yielded [U‐14C]solanesol with a total activity of 474 m̈Ci, a specific activity of 0.5 mCi/mmol, and a radiochemical purity of 95% as determined by RP‐HPLC. The chemical purity was 97% and the chemical identity of the isolated compound was confirmed by co‐chromatography with reference material and by mass spectroscopy.
The preparation of 14C, 35S and 13C labelled forms of omeprazole
Authors: Crowe A M , Ife R J , Mitchell M B , Saunders D 
Published: October 2006

AbstractThe syntheses of [benzimidazole‐2‐14C]omeprazole, [benzimidazole‐2‐13C]omeprazole, [35S]omeprazole and [2‐pyridyl‐14C‐methyl]‐omeprazole are described. The first three compounds were prepared from the approprlate isotopically labelled carbon disulphide. The key step in the synthesis of [2‐pyridyl‐14C‐methyl]omeprazole is nucleophilic alkylation of a 1‐ethoxypyridinium salt using [14C]methyl magnesium idodide. This is the first time that a reaction of this type has been used to prepare a 2‐[methyl]‐14C]methylpyridine.
I‐125 and I‐123 labelled iodobenzyl bromide, a useful alkylating agent for radiolabelling biologically important molecules
Authors: Wilson Alan A. , Dannals Robert F. , Ravert Hayden T. , Burns H. Donald , Wagner Henry N. 
Published: October 2006

AbstractThe radioiodination of 4‐trimethylsilylbenzyl bromide in acetic acid with no carrier added I‐125 and I‐123 iodide ion and N‐chlorosuccinimide (NCS) is a rapid, high yielding process which produces high specific activity 4‐[I‐125 or I‐123]iodobenzyl bromide. This radiolabelled alkylating agent has been efficiently reacted with N,N‐dimethylaniline and triphenylphosphine to generate radiolabelled quaternary ammonium and phosphonium salts, and should be useful for labelling other biologically important molecules which possess suitable nucleophilic functional groups.
Synthesis of tritium labelled adinazolam with high specific activity
Authors: Palmer John R. 
Published: October 2006

AbstractTritium labelled 8‐chloro‐1‐[(dimethylamino)methyl]‐6‐phenyl‐4H‐s‐triazolo[4,3‐a][1,4]benzodiazepine was prepared from [3H]bromomethane and 8chloro‐1‐[(N‐methylamino)methyl]‐6‐phenyl‐4H‐s‐triazolo[4,3‐a][1,4]benzodiazepine. The latter compound was efficiently obtained from 8‐chloro‐6‐phenyl‐4H‐s‐triazolo[4,3‐a)[1,4]benzodiazepine by hydroxymethylation, mesylation and mesylate displacement with aqueous methylamine. The titled product had a specific activity of 80 Ci/mmole.
Synthesis of D3‐metoclopramide
Authors: Jamet G. , Kerr Robert R. , Staveris S. , Jung L. , Koffel J. C. 
Published: October 2006

AbstractMetoclopramide‐d3 with the three deuterium atoms in the methoxy function ortho to the benzamide group was synthesized. A previously published synthesis was followed but was extensively modified in the final steps to increase overall yield. Structure was verified by NMR and GC‐MS.
Synthesis and evaluation of fluorinated derivatives of fentanyl as candidates for opiate receptor studies using positron emission tomograpry
Authors: Hwang Dah‐Ren , Feliu Anthony L. , Wolf Alfred P. , Macgregor Robert R. , Fowler Joanna S. , Amett Carroll D. , Holland H. Jean , Carr Kenneth , Simon Eric J. 
Published: October 2006

AbstractThree fluorinated derivatives of fentanyl, fluorofentanyl (3), keto‐fluorofentanyl (5), and fluorofentanol (6), were synthesized and their abilities to compete with 3H‐diprenorphine for binding sites in guinea pig brain membranes were determined. The relative potencies were fentanyl > 3 ∼ 6 ≫ 5. On the basis of its apparent affinity for opiate receptors and its relative ease of synthesis,.6 was selected for further study. Fentanyl was slightly better than.6. in its ability to compete with [3H]naltrexone for binding sites in rat brain membranes. Both fentanyl and 6 exhibited a similar high “sodium ratio” (quotient of the IC50's against [3H]naltrexone in the presence and absence of sodium chloride) generally characteristic of opiate agonists. The analgesic potencies of fentanyl and 6 were determined in rats by measuring suppression of locomotion and vocalization responses to footshock. 6 appeared slightly less potent than fentanyl, but produced a similar analgesia and catalepsy which was entirely blocked by pretreatment of rats with naloxone, an opiate antagonist. A rapid synthesis of [18F]‐6 was developed and the tissue distribution of [18F]‐6 in mice was determined 5, 60, and 120 minutes after intravenous injection. The use of this general route to 18F‐labeled derivatives of fentanyl for studies of the opiate receptor using positron emission tomography is planned.
Synthesis of tritium labelled 7‐dehydrocholesterol 5β,6β‐oxide
Authors: Michaud Dennis P. , Nashed Nashaat T. , Jerina Donald M. 
Published: October 2006

AbstractWe report the synthesis of tritiated 7‐dehydrocholesterol 5β,6β‐oxide in high specific activity. Oxidation of 7α‐bromo‐cholesterol 5β,6β‐oxide to the 3‐keto epoxide followed by borotritide reduction, in a special buffer‐organic solvent system to minimize undesired rearrangement, regenerated the 3β‐hydroxyl group. Base‐assisted elimination produced the title compound.
Synthesis of [14C]zolpidem
Authors: Allen John , Tizot André 
Published: October 2006

AbstractThe synthesis of [14C]Zolpidem, a new hypnotic agent having a non‐benzodiazepine structure, is described. This compound was synthesised in a 64% overall radio‐chemical yield from potassium[14C]cyanide and with a specific radioactivity of 56 mCi/mmol. It was used for pharmacokinetic and drug metabolism studies.
Syntheses of carbon‐14 and sulfur‐35 labeled 2‐(morpholinothio)benzothiazoles and carbon‐14 labeled 2‐(cyclohexylaminothio)benzothiazoles
Authors: Tanaka A , Fukuoka M , Adachi T , Yamaha T 
Published: October 2006

AbstractSome vulcanizing accelerators, mercaptobenzothiazole derivatives labeled with carbon‐14 or sulfur‐35 were prepared. 2‐(Morpholinothio)benzothiazole labeled with carbon‐14 or sulfur‐35 of the sulfhydryl group at position 2 was synthesized by oxidative condensation with sodium hypochlorite from a mixture of morpholine and 2‐mercaptobenzothiazole‐2‐14C or 2‐mercaptobenzothiazole‐2‐35S. The same method was applicable to the synthesis of 2‐(morpholino‐U‐14C‐thio)‐benzothiazole using morpholine‐U‐14C as starting material.
Synthesis of tritium and carbon‐14 labeled 4,5‐bis(4‐methoxyphenyl)‐ 2 ‐(trifluoromethyl)thiazole
Authors: Hsi Richard S. P. , Stolle Wayne T. 
Published: October 2006

AbstractTritium labeled 4,5‐bis(4‐methoxyphenyl)‐2‐(trifluoromethyl)thiazole (1) was synthesized with the tritium label located on the phenyl ring at the C‐4 position of the thiazole ring and meta to the methoxy group. Anisole specifically labeled with tritium at C‐3 was used to prepare tritium labeled 1 with specific activity of 53 μCi/mg in 53% overall radiochemical yield. The title compound 1 was also labeled with carbon‐14 at the C‐4 position of the thiazole ring. [14C)Barium carbonate was used as the isotope source, and carbon‐14 labeled compound 1 of 31.4 μCi/mg was obtained in 54% overall radiochemical yield. Deuterium and carbon‐13 labeled starting materials and intermediates were used as models for preparing the tritium and carbon‐14 labeled compounds, respectively.
Radiolabelling of poly(butyl 2‐cyanoacrylate) nanoparticles with a technetium‐99m‐dextran complex
Authors: Douglas Stephen J. , Davis Stanley S. 
Published: October 2006

AbstractPoly(butyl 2‐cyanoacrylate) nanoparticles have been radiolabelled with a 99mTc‐dextran complex to allow their pattern of biodistribution to be followed by using the technique of gamma scintigraphy. The method involves the preforming of a 99mTc‐dextran complex and using this as a polymerie stabiliser during the formation of nanoparticles. Copolymerisation of this complex with the cyanoacrylate monomer results in the radiolabel being covalently linked to the nanoparticle matrix with a labelling efficiency of approximately 18%. The radiolabelled nanoparticles slowly degrade and release the activity into buffer solution. The release rate was relatively unaffected by the presence of plasma proteins indicating that the system should be suitable for use in vivo.
Marquage par 14C DU S‐Acetyl, N‐Glycylcysteamine (1 102)
Authors: Madelmont J. C. , Moreau M. F. , Godeneche D. , Parry D. , Oiry J. , Imbach J. L. 
Published: October 2006

AbstractLe trifluoroacetate de S Acetyl N glycyl cystéamine a été marqué par 14C en trois positions

Sur le groupe cystéamine par l'intermédiaire de la 14C 1 benzyloxycarbonyl éthanolarnine.
Sur le carbonyl peptidique par l'intermediaire de la 14C I BOC glycine.
Sur le groupe acétyle en utilisant l'anhydride acétique 14C.
Stereochemistry of reductive dehalogenation with deuterium gas
Authors: Kaspersen Frans M. , Sperling Eric M. 
Published: October 2006

AbstractThe stereochemistry of reductive debromination and deiodination of 4‐haloprolines and 2‐ or 7‐bromo‐cholesterols with 2H2 catalyzed by Pd was investigated using 2H NMR. The reactions are stereoselective but not stereospecific.
Radiolysis of D(+)‐carnitine by 60Co‐γ‐radiation and formation of L(+)‐β‐methylcholine
Authors: Löster Heinz , Strack Erich , Seim Hermann 
Published: October 2006

AbstractThe radiolysis of D(+)‐carnitine by 60Co‐γ‐radiation was examined to obtain optically active β‐methylcholine. It was found that the radio lysis leads to a number of trimethylammonium bases but to no other betaines. The acids formed were not investigated. The bases produced were separated by ion exchange chromatography. (+)‐β‐Methylcholine and acetonyltrimethylammonium could be identified by means of common analytical methods (IR, NMR, MS and MA) applied to the fractions. The amounts of methylamines formed by irradiation, and determined by gas chromatography, were very small. Racemization of the D(+)‐carnitine did not occur during irradiation, L(‐)‐carnitine was not found when an enzymatical determination method was used. The fact that (+)‐β‐methylcholine was formed from D(+)‐carnitine is pharmacologically important, because acetyl‐L(+)‐β‐methylcholine has a strong interaction with muscarinic receptors.
Synthesis of [Carbonyl‐14c] labeled carbonate and carbamate esters
Authors: Nassar Munir N. , Agha Bushra J. , Digenis George A. 
Published: October 2006

AbstractA two‐step synthesis of three carbonate and four carbamate esters labeled at the carbonyl with carbon‐14 is described. The method utilizes the readily available [14C]‐phosgene which is first converted to an isolable [14C]‐labeled alkyl or aryl chloroformate and subsequently reacted with the appropriate alcohol or amine to give the corresponding ester.
The preparation of ormetoprim labeled with carbon‐14
Authors: Liebman Arnold A. , Bader Gerhard J. , Kaegi Heinz H. , Perry Clark W. 
Published: October 2006

AbstractThe sulfonamide potentiator ormetoprim (6) has been prepared with a carbon‐14 label for use in biological studies. The key intermediate. 2‐methylveratraldehyde (4), was prepared by 14CO2 carbonation of the Grignard reagent from 2‐bromo‐4,5‐dimethoxytoluene (1) followed by esterification. reduction and manganese dioxide oxidation.
Specifically labelled beta‐carbolines for biomedical investigations
Authors: Gynther J. , Huhtikangas A. , Auriola S. , Juvonen H. 
Published: October 2006

AbstractFive radioactive and three deuterium labelled 1.2,3,4‐tetrahydro‐beta‐carbolines (THBCs) have been synthesized from tryptamine hydrochloride or 5‐methoxytryptamine hydrochloride and formaldehyde, glyoxylic acid or pyruvic acid. Radioactive labelling was performed using [14C] and [3H]labelled compounds. while the deuterium labels were introduced using lithium aluminium deuteride. The specific activities obtained for [14C] labelled THBCs varied between 1.0 and 5.0 mCi/mmol, while a value of 30.1 mCi/mmol was obtained for the tritiated compound. The isotopic purities of the deuterated THBCs were in the range of 76.3 ‐ 96.2 %.
Convenient one‐pot synthesis of benzoquinone‐[U‐14c] and hydroquinone‐[U‐14c]
Authors: Parnes Howard , Dekeczer Steve 
Published: October 2006

AbstractBenzoguinone‐[U‐14C] was synthesized in 90% yield from benzene‐[U‐14C] via a three step seguence. Conditions were developed which allowed this conversion to be accomplished in a one pot closed system. The benzoquinone‐[U‐14C] thus obtained could be reduced to hydroquinone‐[U‐14C] in quantitative yield. Preparation of benzene‐[U‐14C] is also described.
Synthesis of deuterium‐labeled felbamate from diethyl phenylmalonate
Authors: Choi Yong M. , Kucharczyk Norbert , Sofia R. Duane 
Published: October 2006

AbstractA synthesis of felbamate‐d4 (2‐phenyl‐1.3‐propanediol‐1,1,3,3‐d4 dicarbamate) starting from diethyl phenylmalonic acid ester and lithium aluminum deuteride was developed. The procedure has three steps from the starting material to felbamate‐d4 via the intermediate. 2‐phenyl‐1,3‐propanediol‐1,1,3,3‐d4. The final overall yield was 44%. The isotope purity was 99.2%.
Synthesis and biodistribution of radioiodinated selenonium salts: Potential myocardial imaging agents
Authors: Parikh A. S. , Basmadjian G. P. , Gilliland D. L. , Greenwood R. B. , Rieger J. A. , Weaver A. 
Published: October 2006

Abstract(o‐[125I]iodobenzyl)benzylmethylselenonium tetrafluoroborate (1) and (o‐[125I]iodobenzyl)dibenzylselenonium tetrafluoroborate (2) were synthesized by methylation and benzylation of o‐[125I]iodobenzyl benzyl selenide respectively. The starting compound o‐iodobenzyl benzyl selenide was radioiodinated with sodium [125I]iodide by melt‐exchange in a sealed ampoule maintained at 75°C for 12 hours, with subsequent chromatographic purification yielding the pure compound in a radiochemical yield of 33.0% and specific activity of at least 68.0 mCi/mmol. Tissue distribution studies of compounds 1 and 2, performed in rats, showed that the labelled compounds accumulated rapidly in the heart. The maximum heart‐to‐blood ratios for compounds 1 and 2 were 4.2:1 and 4.4:1 compared to that of 2.0:1 for previously synthesized [75Se]Trimethylselenonium Iodide (3).
Catalytic dehalogenation of N‐acetyl‐L‐4‐chloro‐ and N‐acetyl‐L‐4‐iodophebylalanine amide in the presence of deuterium
Authors: Oehlke J. , Bienert M. , Niedrich H. , Zöpfl H.‐J. , Franke P. 
Published: October 2006

AbstractAs a model for the tritium labeling of peptides, the catalytic dehalogenation of N‐Acetyl‐L‐4‐chloro‐ and N‐Acetyl‐L‐4‐iodo‐phenylalanine amide was investigated in the presence of deuterium, using different reaction conditions. A catalyst‐mediated transfer of the solvent‐hydrogen to the substrate was found to be the most probable reason for the exchange of halogen by hydrogen instead of deuterium. This unwanted transter was most intensive in the presence of water. An incorporation of additional deuterium besides the 4‐position of phenylalanine takes place simultaneously with the dehalogenation especially of the chloro derivative.
Synthesis of disodium (+)‐(Z)‐[[[1‐(2‐amino‐4‐[2‐14c]thiazolyl)2‐[[(2s,3s)‐2‐(carbamoyloxymethyl)‐4‐oxo‐1‐sulfonato‐3‐azetidinyl]amlno]‐2‐oxoethylidene]amino]oxy]acetate
Authors: Imanishi M. , Tomimoto M. , Watanabe M. , Hayashi N. 
Published: October 2006

AbstractDisodium (+)‐(Z)‐[[[1‐{2‐amino‐4‐[2‐14C]thiazolyl)‐2‐[[ (2S,3S)‐2‐(carbamoyloxymethyl)‐4‐oxo‐1‐sulfonato‐3‐azetizinyl]amino‐2‐oxoethylidene]amino]oxy]acetate ([14C]AMA‐1080) was synthesized via [2‐(2‐chloroacetamido‐4‐[2‐14C]thiazoiyl)‐(Z)‐2‐(4‐nltrobenzyloxycarbonylmethoxyimino)]acetic acid from [14C]thiourea. Trisodium (+)‐(Z)‐[[[1‐(2‐amino‐4‐[2‐14C]thiazoiyl)‐2‐[[(1S, 2S)‐3‐carbamoyloxy‐1‐carboxylato‐2‐sulfonato‐aminopropyl]amino]‐2‐oxoethylidene]amino]oxy]acetate ([ 14C]AMA ‐1294) as the principal metabolite of [14C]AMA‐1080 was also prepared.
Synthesis of NO‐carrier added 11C‐labelled [methyl]choline analogs
Authors: Diksic Mirko , Jolly Dean 
Published: October 2006

AbstractWe describe here the synthesis of two[11C‐methyl]labelled analogs of choline and the influence of the solvent, addition of a base, and reaction time on the radiochemical yield. The reactions produced equally good yields in methanol and acetonitrile and reached maximum radiochemical yield at about 5‐10 min. The addition of a base in the case of [11C‐methyl]pyrrolidinocholine increases the radiochemical yield. Optimum radiochemical yields were 30% for[11C‐methyl]piperidinocholine and 40% for[11C‐methyl]pyrrolidinocholine for two choline analogs.
Synthesis of 7α‐chloro‐16α‐methylprednisolone 17α,21‐dipropionate‐4‐14c (alclometasone dipropionate‐4‐14c)
Authors: Terasawa Tadao , Atsumi Kazunori , Yokoshima Tetsuyoshi , Ohyabu Shintaro , Fukasaku Noboru 
Published: October 2006

AbstractGrignard reaction of the enol‐lactone 8 with 14C‐methylmagnesium iodide afforded an adduct 9 which on subsequent treatment with lithium 2,6‐di‐t‐butylphenoxide gave the enone 10. Conversion of 10 to the trienone 12 was performed by two‐step dehydrogenation using chloranil and then DDQ. The protecting groups were removed on treatment whith 2N‐hydrochloric acid‐trifluoroacetic acid to give the triol 13. The 17α,21‐bisesterification of 13 was carried out according to the orthoester procedure. Finally, addition of dry hydrogen chloride to the resulting diester 16 led to the title compound 17.
A practical preparative scale synthesis of d/l‐6‐fluorodopa
Authors: Grierson J. R. , Adam M. J. 
Published: October 2006

AbstractA practical preparative scale synthesis of D/L‐6‐fluorodopa (6‐FD) is presented. From veratric acid the procedure affords D/L‐6‐FD in 12% overall yield in 11 steps. Useful batch quantities ( > 300 mg) of this material were readily obtained and used as an analytical standard for 19F NHR and HPLC analyses in the preparation of L‐[18F]6‐fluorodopa.
Synthesis of tritium labeled 2,3,4,5‐tetrahydro‐1H‐3‐benzazepines
Authors: Landvatter Scott W. , Blackburn Dale W. , Villani Anthony J. , Bosch Gregory K. 
Published: October 2006

AbstractSKF 82526 (6‐chloro‐7,8‐dihydroxy‐1‐(4‐hydroxyphenyl)‐2,3,4,5‐tetrahydro‐1H‐3‐benzazepine) has been synthesized in both racemic mono and enantiomerically pure ditritiated form; SKF 38393 (7,8‐dihydroxy‐1‐phenyl‐2,3,4,5‐tetrahydro‐1H‐3‐benzazepine) has also been labeled with tritium. In each case labeling was accomplished via tritiation of the appropriate ring halogenated precursor with tritium gas over Pd catalyst in triethylamine in DMF.
Synthesis of 4‐13C and 3,5‐13C labeled aniline as precursor of 13C ‐ labeled monosubstituted benzenes
Authors: Rumpel Helmut , Limbach Hans‐Heinrich 
Published: October 2006

AbstractAniline (IV), specifically 13C labeled in the 4‐ or in the 3,5‐position (IVa and IVb), has been synthesized with 55% yield from 13C labeled p‐nitrophenol (II). The reduction of the NO2 group and the removal of the OH group was performed in one step by reduction and hydrogenolytic cleavage of p‐nitrophenol‐methanesulfonate (III), prepared in 90% yield from (II). From (IV) a number of specifically 13C labeled monosubstituted benzenes C6H5Y (Y = CN, Hal, NO2) are easily accessible.
Preparation and purification of [14C] labeled N‐demethyl lincomycin and propylproline from [14C] tyrosine
Authors: Hausknecht E. C. , Wolf H. J. 
Published: October 2006

AbstractPropylproline and N‐demethyl‐lincomycin, two intermediates in lincomycin biosynthesis, were prepared in radiolabeled form. [14C]‐labeled N‐demethyl‐lincomycin was synthesized by a resting cell suspension of a lincomycin negative mutant of Streptomyces lincolnensis that was fed methylthiolincosaminide and uniformly labeled [14C]‐tyrosine. [14C]‐N‐demethyl‐lincomycin was isolated from the culture medium by ion exchange chromatography and reverse phase‐ion pair high pressure liquid chromatography. [14C]‐propylproline was generated by the base hydrolysis of [14C]‐N‐demethyl‐lincomycin and isolated by anion exchange chromatography. The products had radiochemical purities greater than 95% and specific activities of 5.9 mCi/mmole.
New N‐permethylations and introduction of deuterium labelled methyl groups into primary and secondary amines
Authors: Giumanini Angelo G. , Verardo Giancarlo , Gei Maria H. , Lassiani Lucia 
Published: October 2006

AbstractThe extension of the N‐permethylation reaction of amines to aromatic amines with strong electron withdrawing substituents in o‐ and p‐ positions is reported. A comparison of this method with other “best” last step synthetic methods reported in literature is given. The reaction could be extended to the syntheses of N‐permethyl‐derivatives of amines of the type CH3‐nDn by use of formaldehyde, dideuteroformaldehyde, sodium borodeuteride and ‐hydride. Label conservation in the reaction is complete: the final step in the reaction involves H− (or D−) transfer from the reducing agent to a reactive species. The MS of the labelled compounds revealed extensive label excange in the ionization chamber. A new homogeneous procedure for the N‐permethylation, especially suited for larger scale preparations, is described.
A convenient synthesis of carbon‐13 labeled 1‐keto‐7‐methoxyoctahydrophenanthrene
Authors: Mohammadi Mohammad , Kabalka George W. , Finn Ronald D. 
Published: October 2006

AbstractCarbon‐13 labeled 1‐keto‐7‐methoxy‐1,2,3,4,9,10,11,12‐octahydrophenathrene (III) and 1‐keto‐7‐methoxy‐2‐methyl‐1,2,3,4,9,10,11,12‐octahydrophenanthrene (IV) were prepared in good yields via the cyanidation of an organoborane.
Synthesis of deuterium labeled 1,3‐dimethyluric acid
Authors: Mamada Kumiko , Furuta Takashi , Kasuya Yasuji 
Published: October 2006

AbstractA synthetic procedure for 1,3‐di(trideuteromethyl)uric acid is described. Deuterium labeling of the N‐1 and N‐3 positions was achieved by methylation of 4‐amino‐5‐carbethoxyuracil with di(trideuteromethyl)‐sulfate followed by cyclization of the dimethylated intermediate by heating. The synthesis resulted in a product with 99.4% d6 isotopic purity, which is selectively deuterated in the methyl groups at the N‐1 and N‐3 positions and chemically pure.
Synthesis and 1H‐nmr of deuterium labeled D,L‐homoserine lactone hydrochlorides
Authors: Ramalingam Kondareddiar , Woodard Ronald W. 
Published: October 2006

AbstractThe synthesis of six regiospecific deuterated D,L‐homoserine lactone hydrochlorides from the appropriately deuterated 2‐bromo‐1‐(tetrahydropyranyloxy) ethanes which were obtained by reduction of the corresponding ethyl bromoacetates are described. The proton nmr of each lactone is recorded and the chemical shift and coupling constants are reported.
The preparation and characterization of (±)‐[phenoxy‐3H(N)] phenoxybenzamine hydrochloride at high specific activity
Authors: Filer Crist N. , Fazio Robert , Morrison John , Ahern David G. 
Published: October 2006

Abstract(±)‐Phenoxybenzamine is a ligand capable of irreversibly alkylating the alpha‐1 adrenergic receptor. Previous attempts to radiolabel it have achieved only low specific activities which impeded their use in neurochemical investigations. (±)‐[Phenoxy‐3H(N)] Phenoxybenzamine.HCL (1) has been prepared in our laboratory by the catalytic reductive aryl debromination of an appropriate brominated precursor with tritium gas. 3H NMR showed exclusive radiolabeling on the phenoxy ring and the radioligand had a specific activity of 32.4 Ci/mmol.