Synthesis method of isotope labeled dansyl chloride-13C2

An isotope labeling, dansyl chloride technology, applied in the preparation of sulfonic acid, organic chemistry, etc., can solve the problems of large consumption of sodium bicarbonate, large environmental impact, and material flushing, and achieve simplified post-processing, improved safety, and safe operation. handy effect
CN104945285AInactive Publication Date: 2015-09-30无锡贝塔医药科技有限公司
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
无锡贝塔医药科技有限公司
Publication Date
2015-09-30
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention relates to a synthesis method of isotope labeled dansyl chloride-13C2. The synthesis method is characterized by comprising the following steps: dissolving dansyl acid-13C2 in a solvent, cooling to 0 DEG C under nitrogen protection, dropwise adding anhydrous N,N-dimethylformamide and further dropwise adding a chlorination reagent; after the dropwise adding operation is finished, heating to the range of 30-70 DEG C and reacting for 2-5 hours; after the reaction is finished, cooling the solution to a room temperature, removing the solvent and the chlorination reagent by virtue of reduced-pressure distillation, adding ice water to the residue while stirring, and then adding sodium bicarbonate to regulate the pH value to the range of 5-7, extracting organic phases by use of dichloromethane or ether, mixing the organic phases, orderly washing by use of water and saturated salt water, drying the organic phase by use of anhydrous magnesium sulfate, and then filtering, concentrating and drying to obtain the crude product of the isotope labeled dansyl chloride-13C2. The synthesis method of the isotope labeled dansyl chloride-13C2 has the advantages of safe operation, good convenience and relatively high yield.
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Description

technical field

[0001] The invention relates to a method for synthesizing isotope-labeled dansyl chloride-13C2. Background technique

[0002] Liquid chromatography coupled to mass spectrometry (LC / MS) has become a very important tool in metabolic research. An ideal LC / MS platform will identify and quantify all metabolites present in biological samples such as cell extracts and biological fluids. Unfortunately, it is very challenging to detect all metabolites at once due to the large differences in the chemophysical properties of the metabolites.

[0003] One strategy to address this diversity is to divide metabolomes into groups based on hydrophobicity, chemical structure, or other attributes, and then use several tailor-made optimized LC / MS methods to target each metabolome. Group metabolites were analyzed.

[0004] However, we can also look for an analysis strategy for selectively labeling metabolites based on the fact that the metabolites contain certain chemical funct...

Claims

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