A practical procedure of synthesis of tritium labeled troglitazone

Journal of Labelled Compounds and Radiopharmaceuticals

Volumn 53, Issue 5-6, 2010, Pages 441-442

  Tang, Yui S ^a   Liu, Wensheng ^a   Braun, Matthew P ^a   Ho, Jonathan Z ^a  

^a MERCK RESEARCH LABORATORIES   (United States)

Author keywords

Iodination; Tritium labeling; Troglitazone

Indexed keywords

HALOGENATION;

IODINATION; LABELINGS; PRACTICAL PROCEDURES; TRITIATION; TRITIUM LABELING; TROGLITAZONE;

TRITIUM;

IODINE DERIVATIVE; N IODOSUCCINIMIDE; PIOGLITAZONE; ROSIGLITAZONE; TRITIUM; TROGLITAZONE; UNCLASSIFIED DRUG;

ANIMAL EXPERIMENT; ANIMAL MODEL; CATALYSIS; CONFERENCE PAPER; CONTROLLED STUDY; DRUG STRUCTURE; DRUG SYNTHESIS; IODINATION; ISOTOPE LABELING; LOW TEMPERATURE; NONHUMAN;

EID: 77955132340     PISSN: 03624803     EISSN: 10991344     Source Type: Journal    
DOI: None     Document Type: Conference Paper

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10. 5) was added, and the brown suspension was filtered through a syringe-less filtering devise to remove solid. MeOH (1 mL) was used to rinse the solid and combined filtrate was concentrated under vacuum to give an oil which was purified by Reverse Phrase HPLC (Luna C8 column, 22.5 x 250 mm) with an isocratic eluent of MeCN:water:TFA = 30:70:0.1 at a flow rate of 10 mL/min.
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12. 3 (5 mg) in anhydrous DMF (0.8 ml) was degassed and stirred at to 0°C for 5 min. A carrier-free tritium gas (1.2 Ci) was introduced under vacuum of 240mm Hg, and the resulting mixture was stirred at 0°C for 2 h. Excess tritium gas was removed, and the mixture was filtered through a syringe-less filter device (0.45 um, polytetrafluoroethylene; autovial; Whatman, Clifton, NJ). The filtrate was concentrated under vacuum to give an oil. EtOH (2 mL) was added to make a solution which was purified by HPLC (Phenomenex Luna Phenyl-Hexyl column, 9.4mm x 250 mm, Torrance, CA) with a gradient eluent of MeCN:water:TFA from 25:75:0.1 to 30:70:0.1 in 50 min at a flow rate of 10 mL/min.The product 3c was collected at the retention time of 28 min (25 mCi; 23 Ci/mmol, radiochemical purity >99%). The identity was confirmed by LC/MS analysis and HPLC co-elution with unlabeled reference sample.