PRODUCTION OF PET PRECURSOR Russian patent published in 2016 - IPC C07B59/00 C07C227/40 C07C269/08 C07C271/24 C07C303/28 

FIELD: chemistry.

SUBSTANCE: invention relates to a method for producing a compound of formula IIIa, where R is an alkyl group with 1-5 carbon atoms; X is a protecting group for an alcohol selected from benzyl (Bn), methoxymethyl (MOM), 2-methoxyethoxymethyl (MEM), methylthiomethyl (MTM), tetrahydropyranyl (THP), benzyloxymethyl (BOM), p-methoxyphenyl, p-methoxybenzyl (MPM ), p-methoxybenzyloxymethyl (PMBM), triisopropylsilyl (TIPS), tert-butyldimethylsilyl (TBDMS), 2-(trimethylsilyl) ethoxymethyl (SEM), and (phenyldimethylsilyl)methoxymethyl (SMOM); Y is a protecting group for an amine selected from tert-butylcarbamate (Boc), 9-fluorenylmethylcarbamate (Fmoc), methyl carbamate, ethyl carbamate, 2-chloro-3-indenylmethylcarbamate (Climoc), benz[f]inden-3-ylmethylcarbamate (Bimoc) 2,2,2-trihloretilkarbamata (Troc), 2-chlorethylcarbamate, 1,1-dimethyl-2,2-dibromethylcarbamate (DB-t-BOC), 1,1-dimethyl-2,2,2-trichlorethylcarbamate (TCBOS) benzylcarbamate (Cbz) and diphenylmethylcarbamate. Disclosed method comprises a processing method comprising steps of 1)-5). At step 1) providing a crude reaction product comprising said compound of formula IlIa; 2) adding ethyl acetate to crude reaction product of step (1) to obtain a suspension;3) adding water to suspension of step (2) to form a biphasic system comprising an aqueous phase and an organic phase, and discarding aqueous phase;4) adding an acid to organic phase of step (3) to form a biphasic system comprising an acidic aqueous phase and an organic phase, and discarding acidic aqueous phase;5) washing organic phase of step (4) with water. Invention also relates to methods of producing compounds of formulae Va and VI and can be used in synthesis of radiopharmaceutical precursors for positron emission tomography.

EFFECT: proposed method enables to avoid formation of emulsions during synthesis on an industrial scale and obtain a diphasic system with good separation.

14 cl, 1 ex