Determination method of (2s,5r)-phenoxyaminopiperidine-2-carboxylate ethyl oxalate

Abstract

The invention discloses a (2S, 5R)-5-methyl-5-[(benzyloxy)amino]piperidine-2-carboxylate ethanedioate detecting method. The (2S, 5R)-5-methyl-5-[(benzyloxy)amino]piperidine-2-carboxylate ethanedioatedetecting method implements detection through a high performance liquid chromatograph, performs quantitative analysis through area normalization; applied chromatographic conditions comprise that an applied chromatographic column is chiralcel AD-H; the sample size is 15-25 mu l; the flow velocity is 0.8-1.2 ml / min; the column temperature is 10-40 DEG C; the detection wavelength is 208-212 nm; normal hexane and absolute ethyl alcohol serve as moving phase at a volume ratio of 820-880:150; normal hexane, absolute ethyl alcohol and diethylamine serve as diluent at a volume ratio of 80-90:10-20:1;an ultraviolet detector serves as the detector. The (2S, 5R)-5-methyl-5-[(benzyloxy)amino]piperidine-2-carboxylate ethanedioate detecting method can achieve rapid and accurate measurement of (2S, 5R)-5-methyl-5-[(benzyloxy)amino]piperidine-2-carboxylate ethanedioate and is high in sensitivity, simple in operation and capable of achieving full separation and providing a basis of research, development and quality detection for studying (2S, 5R)-5-methyl-5-[(benzyloxy)amino]piperidine-2-carboxylate ethanedioate compounds.

Description

technical field [0001] The invention relates to a detection method of an avibactam sodium intermediate, belongs to the technical field of drug analysis, and specifically relates to a detection method of (2S, 5R)-phenoxyaminopiperidine-2-ethyl carboxylate oxalate. Background technique [0002] (2S,5R)-Phenoxyaminopiperidine-2-carboxylic acid ethyl ester oxalate, its CAS number is 1416134-48-9, is an important intermediate in the production of Avibactam sodium (Avibactam), its chiral Purity and isomer impurities directly affect the chiral purity of avibactam sodium and the amount of isomer impurities, thereby directly affecting the curative effect of avibactam sodium. [0003] Chemical name of avibactam sodium: [(1R,2S,5R)-2-(aminocarbonyl)-7-oxo-1,6-diazabicyclo[3.2.1]oct-6-yl]sulfuric acid Monoester, which belongs to diazabicyclooctone compound, is currently the most promising new type of β-lactamase inhibitor. Compared with the three marketed β-lactamase inhibitors, it ha...

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Problems solved by technology

[0004] At present, there are no relevant literatures and reports on the detection method of chiral purity of (2S,5R)-phenoxyaminopiperidine-2-carboxylate ethyl oxalate, in order to strengthen (2S,5R)-phenoxyamino For quality control of ethyl piperidine-2-carboxylate oxalate, it is necessary to develop a detection method for (2S,5R)-phenoxyaminopiperidine-2-ethyl carboxylate oxalate, especially the detection of its chiral purity method

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