摘要:

Abstract[Fluorophenyl‐3H(N)] Ocfentanil (1b) and [fluorophenyl‐3H(N)] brifentanil [2b] were synthesized by catalytic tritiation of appropriate bromo precursors (1a, 2a). The products were purifled by preparative HPLC and characterized chromatographically and by proton decoupled3H

ISSN:0362-4803    

DOI:10.1002/jlcr.2580361102

出版商:John Wiley&Sons, Ltd.    

年代:1995

数据来源: WILEY

摘要:

Abstract2‐Amino‐3,5‐dihydro‐7‐(3‐thienylmethyl)‐[6‐14C]‐4H‐pyrrolo [3,2‐d]pyrimidin‐4‐one monohydrochloride ([14C]Cl‐1000), a potent purine nucleoside phosphorylase inhibitor, was made in six steps from potassium [14C]cyanide. A key step was the reduction of a nitro and a nitrile group with sodium hypophosphite and RaNi followed by cyclization of the resulting intermediate to form a

ISSN:0362-4803    

DOI:10.1002/jlcr.2580361103

出版商:John Wiley&Sons, Ltd.    

年代:1995

数据来源: WILEY

摘要:

AbstractThe experimental conditions which control the exchange from deuterium or tritium gas into the C‐1 proton position of glucose in aqueous solution have been studied in detail, with a view to determining the factors which maximize exchange into glucose, but minimize exchange into the solvent water. The favoured conditions for producing glucose with close to 100% isotope labelling in the C‐1 position, and with negligible formation of labelled byproducts, were a reaction time of 6 to 8 hours, a temperature of 60 °C, and a pH of 7 or higher. Pd/BaSO4was the preferred catalyst and slow pre‐addition of the deuterium or tritium gas to the catalyst bed was essential to maximize the subsequent isotope exchange into the sub

ISSN:0362-4803    

DOI:10.1002/jlcr.2580361104

出版商:John Wiley&Sons, Ltd.    

年代:1995

数据来源: WILEY

摘要:

AbstractA new dopamine D2‐like receptor ligand, (R,S)trans‐5‐hydroxy‐2‐[N‐n‐propyl‐N‐(3′‐iodo‐2′‐propenyl)amino]tetralin ((R,S)trans‐5‐OH‐PIPAT,3), based on high affinity dopamine receptor agonist 5‐hydroxy‐2‐[N,N‐(di‐n‐propyl)‐2‐amino]tetralin (5‐OH‐DPAT,1). was prepared. The synthesis was achieved by a reductive amination of 5‐methoxy‐2‐tetralone with n‐propylamine, followed by N‐alkylation, to afford 5‐methoxy‐N‐propyl‐N‐2′‐propynyl‐2‐aminotetralin,7. Reduction of7with tributyltin hydride gave the tri‐n‐butyl tin derivative,8, which was converted to9by an iododemetalation reaction. Demethylation of9gave the desired compound, (R,S)trans‐5‐OH‐PIPAT,3. The resolved (R) and (S)trans‐5‐OH‐PIPAT,3were also quantitatively prepared.In vitrobinding studies showed the stereoselectivity of this new compound for binding to dopamine D2‐like receptors.S(‐)‐3displayed high binding affinity, with inhibition constants (Ki) of 0.38, 0.09 and 0.67 nM for dopamine D2H (expressed in HEK293 cells), D3 (expressed in Sf9 cells) and D4H receptors (expressed in CHO cells), respectively. Using the same binding assays, the less activeR(+) isomer displayed Kivalues of 7.29, 4.87 and 16.44 nM for D2H, D3 and D4H receptors, respectively. In addition, radiolabeling was successfully performed, either with the racemic tin derivative, (R,S)‐11, or using the optic

ISSN:0362-4803    

DOI:10.1002/jlcr.2580361105

出版商:John Wiley&Sons, Ltd.    

年代:1995

数据来源: WILEY

摘要:

Abstract[10‐3H]Farnesol ((2E,6E)‐3,7,11‐trimethyl‐2,6,10‐dodecatrien‐1‐ol) and [10‐3H]farnesal ((2E,6E)‐3,7,11‐trimethyl‐2,6,10‐dodecatrien‐1‐al) were synthesized by sequential reduction and oxidation of the correspondingtert‐butyldiphenylsilyl protected 11,12,13‐trisnoraldehyde, followed by Wittig homologation using isopropyltriphenylphosphorane. Direct reduction of the C‐12 allylic bromide or allylic chloride proved to be an nonviable method, resulting in either multiple decomposition products or significant double bond transposition. Oxidation of the [10‐3H]labelled trisnoralcohol with pyridinium chlorochromate resulted in essentially complete retention of the radiolabel as was established for the corresponding deuterated material. [3H]labelled farnesol and farnesal were obtained in 78% and 74% yields, respectively, from the trisnoraldehyde. These materials were used as radiotracers for examining the enzymatic activity of insect farnesol and farnesal dehydrogenase, key enzymes in t

ISSN:0362-4803    

DOI:10.1002/jlcr.2580361106

出版商:John Wiley&Sons, Ltd.    

年代:1995

数据来源: WILEY

摘要:

AbstractDisodium [benzene‐U‐14C]‐(4‐chlorophenylthio)methylenediphosphonate, [benzene‐14C]‐Tiludronate,2, has been prepared in six steps from [benzene‐U‐14C]‐acetanilide in an overall radiochemical yield of 41%. A key step in this transformation was the efficient conversion of [U‐14C]‐4‐chloroaniline to [benzene‐U‐14C]‐4‐chlorophenylthiocyanate,5, in 83% yield by treatment of the corresponding diazonium salt,9, with iron (III) thiocyanate. It should be noted that formation of the isomeric [benzene‐U‐14C]‐4‐chlorophenylisothiocyanate,11, as a byp

ISSN:0362-4803    

DOI:10.1002/jlcr.2580361107

出版商:John Wiley&Sons, Ltd.    

年代:1995

数据来源: WILEY

摘要:

Abstract[3‐18O]‐L‐serine, [3‐13C]‐L‐serine, [3‐18O]‐L‐threonine, [3,4‐13C2]‐L‐threonine and [3‐2H]‐L‐threonine are prepared from simple commercially available, isotopically enriched starting materials like H218O, [13C]‐paraformaldehyde, [13C2]‐acetaldehyde and [1‐2H]‐acetaldehyde. The introduction of the side chain is based on the reaction of the anion of the bislactimether of cyclo‐(D‐Val‐Gly) with a suitable reagent. For serine this is isotopically labelled benzylchloromethylether, whereas for threonine labelled acetaldehyde is used in combination with chlorotitaniumtris[diethylamide], introducing both stereocentres in one single step. The isotopomers of serine and threonine are obtained on the gram scale in good yields and high enantiomeric and diasteriomeric excesses. New syntheses for [18O]‐benzylalcohol and isotopically enriched benzylchloromethylether are reported. Following the presented synthetic scheme these amino acids can be labelled at an

ISSN:0362-4803    

DOI:10.1002/jlcr.2580361108

出版商:John Wiley&Sons, Ltd.    

年代:1995

数据来源: WILEY

摘要:

AbstractC‐14 labeled (±) 15‐Deoxyspergualin trihydrochloride, 1‐amino‐19‐(14C‐guanidine)‐11‐hydroxy‐4,9,12‐triazanonadecane‐10,13‐dione trihydrochloride was prepared in a 3% overall yield from Carbon‐14 labeled S‐Methyl isothiourea hemisulfate, [imino‐14C]. The radiochemical purity of the sample was 97.0% and the specific ac

ISSN:0362-4803    

DOI:10.1002/jlcr.2580361109

出版商:John Wiley&Sons, Ltd.    

年代:1995

数据来源: WILEY

摘要:

AbstractAn antigastric cancer monoclonal antibody, 3H11 and its Fab fragment, were labelled with a‐emitter211At using p‐(211At)‐astatobenzoic acid (pAtBA) intermediate, in the yields of more than 30%. The astatinated antibodies were stable in vitro, and had specific immunoreactivity to human gastric cancer cell M85. The therapeutic effect of the astatinated antibodies for subcutaneous xenografts of human gastric cancer were investigated in nude mice by i. p. injection,once every 5 days for 3 times sucessively, with 1.48 × 104and 2.22 × 104Bq/g of211At‐3H11 and211At‐3H11 Fab per injection, respectively. It was showed that the volume and weight of xenografts in all tested groups were much smaller and lighter than that of control group (PBS) from 12.5 days post first injection. The most evident inhibition was observed in the groups with211At‐3H11 Fab, with tumor inhibility of 67.5‐69.5% at 15 days and 70.7‐72.3% at 20 d

ISSN:0362-4803    

DOI:10.1002/jlcr.2580361110

出版商:John Wiley&Sons, Ltd.    

年代:1995

数据来源: WILEY

摘要:

Abstract1,2‐anhydroglucitol‐6P, a known inhibitor of glucose‐6P isomerase, behaved as a fructose‐6P site‐directed irreversible inhibitor of bacterial glucosamine‐6P synthase. The lack of reproducibility of the aldolase‐mediated condensation of dihydroxyacetone phosphate and glycidaldehyde followed by borohydride reduction previously described prompted us to develop a chemical route to this compound and its radiolabelled counterpart. The compound was synthesized in 13 steps from D‐arabinose with a 6% overall yield. Tritium introduction was performed at step 11 (3→4) allowing isolation of the title compound of high speci

ISSN:0362-4803    

DOI:10.1002/jlcr.2580361111

出版商:John Wiley&Sons, Ltd.    

年代:1995

数据来源: WILEY