CPC C07D 471/08 (2013.01) [A61K 31/407 (2013.01); A61K 31/4162 (2013.01); A61K 31/427 (2013.01); A61K 31/43 (2013.01); A61K 31/437 (2013.01); A61K 31/439 (2013.01); A61K 31/444 (2013.01); A61K 31/4545 (2013.01); A61K 31/5377 (2013.01); A61K 31/545 (2013.01); A61K 31/546 (2013.01); A61K 45/06 (2013.01); C07D 211/60 (2013.01); C07F 7/0812 (2013.01); Y02P 20/55 (2015.11)] | 9 Claims |
1. A process for preparing (2S,5R)-N-(2-aminoethoxy)-7-oxo-6-(sulfooxy)-1,6-diazabicyclo [3.2.1] octane-2-carboxamide represented by the following formula (III-059):
![]() which comprises:
(i) among the compounds represented by the following formulae (IV-a2), (IV-a3) and (IV-a4):
![]() wherein in the formula (IV-a2), (IV-a3) or (IV-a4), TFA represents trifluoroacetyl, Boc represents tert-butoxycarbonyl, Teoc represents 2-trimethylsilylethoxycarbonyl, and OBn represents benzyloxy, (ia) subjecting to coupling the compound represented by the formula (IV-a2) or (IV-a4) with tert-butyl 2-(aminooxy) ethylcarbamate in the presence of an active ester, an active amide or a dehydration condensing agent, or (ib) subjecting to coupling the compound represented by the formula (IV-a3) with benzyl 2-(aminooxy) ethylcarbamate in the presence of an active ester, an active amide or a dehydration condensing agent, to prepare a compound represented by the following formula (IV-b2-Boc-059), (IV-b3-Cbz-059) or (IV-b4-Boc-059):
![]() wherein in the formula (IV-b2-Boc-059), (IV-b3-Cbz-059) or (IV-b4-Boc-059), TFA represents trifluoroacetyl, Boc represents tert-butoxycarbonyl, Cbz represents benzyloxycarbonyl, Teoc represents 2-trimethylsilylethoxycarbonyl, and OBn represents benzyloxy,
(iia) deprotecting the trifluoroacetyl group of the compound represented by the formula (IV-b2-Boc-059) by a treatment with a base to prepare a compound represented by the following formula (IV-c-Boc-059):
![]() wherein in the formula (IV-c-Boc-059) or (IV-c-Cbz-059), Boc represents tert-butoxycarbonyl, Cbz represents benzyloxycarbonyl, and OBn represents a benzyloxy, or (iib) removing the tert-butoxycarbonyl of the compound represented by the formula (IV-b3-Cbz-059) by an acid treatment to prepare a compound represented by the formula (IV-c-Cbz-059), or (iic) removing the 2-trimethylsilylethoxycarbonyl of the compound represented by the formula (IV-b4-Boc-059) by a fluoride to prepare a compound represented by the formula (IV-c-Boc-059);
(iii) then, after silylating the compound (IV-c-Boc-059) or (IV-c-Cbz-059), carrying out an intramolecular urea formation reaction to prepare a compound represented by the following formula (IIa-Boc-059) or (IIa-Cbz-059):
![]() wherein in the above formula (IIa-Boc-059) or (IIa-Cbz-059), Boc represents tert-butoxycarbonyl, Cbz represents benzyloxycarbonyl, and OBn represents benzyloxy;
(iva) removing the benzyl of the benzyloxy at the 6-position of the compound represented by the formula (IIa-Boc-059) in the presence of a hydrogenolysis catalyst under a hydrogen atmosphere, or (ivb) removing the benzyl of the benzyloxy at the 6-position of the compound represented by the formula (IIa-Cbz-059) in the presence of a hydrogenolysis catalyst under a hydrogen atmosphere, and simultaneously carrying out a tert-butoxycarbonylation in the presence of di-tert-butoxydicarbonate to prepare a compound represented by the following formula (IIb-Boc-059):
![]() wherein in the formula (IIb-Boc-059), Boc represents tert-butoxycarbonyl,
(v) sulfating the hydroxyl group at the 6-position of the formula (IIb-Boc-059) to prepare a compound represented by the following formula (III-Boc-059):
![]() wherein in the formula (III-Boc-059), Boc represents tert-butoxycarbonyl, and M represents H, pyridinium, sodium or tetrabutylammonium; and
(vi) deprotecting the tert-butoxycarbonyl group by an acid treatment.
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