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Synthetic method for stable isotope labeled N,N-dimethylaminochloropropane hydrochloride

A dimethylaminochloropropane, isotope labeling technology, applied in the preparation of amino compounds, chemical instruments and methods, preparation of amino-substituted functional groups, etc. Inapplicability and other problems, to achieve the effects of good economy and practical application value, simple post-processing purification process, and high atom utilization rate

Active Publication Date: 2015-04-01
SHANGHAI RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The natural abundance N,N-dimethylaminochloropropane hydrochloride is mainly obtained by reacting 1,3-bromochloropropane with dimethylamine. Due to the physical and chemical properties of the stable isotope-labeled dimethylamine raw material and The state is unstable, and isotope-labeled raw materials are difficult to obtain, so this synthesis process is not suitable for the synthesis of stable isotope-labeled compounds

Method used

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  • Synthetic method for stable isotope labeled N,N-dimethylaminochloropropane hydrochloride
  • Synthetic method for stable isotope labeled N,N-dimethylaminochloropropane hydrochloride
  • Synthetic method for stable isotope labeled N,N-dimethylaminochloropropane hydrochloride

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Embodiment 1

[0034] a stable isotope 13 C mark N, the synthetic method of N-dimethylaminochloropropane hydrochloride, the specific synthetic process of this method comprises the following steps:

[0035] In a three-neck flask equipped with a magnetic stirrer, a thermometer and a reflux condenser, the isotope 13 The methyl iodide of C mark and chlorpromamine hydrochloride are added in the there-necked flask in molar ratio 1:1, then add the catalyst tetrabutylammonium bromide of 1mol% (calculated as chlorpromamine hydrochloride) and concentration be 25wt% Aqueous sodium hydroxide solution, wherein the molar ratio of sodium hydroxide to chlorpropylamine hydrochloride is 5:1, the solvent is water, react at normal pressure and 35°C for 7 hours; after the reaction is completed, cool to room temperature, and the reaction liquid is separated, After purification, N,N-dimethylaminochloropropane is obtained; dry hydrogen chloride gas is passed into N,N-dimethylaminochloropropane, and stable isotope-...

Embodiment 2

[0037] a stable isotope 13 C mark N, the synthetic method of N-dimethylaminochloropropane hydrochloride, the specific synthetic process of this method comprises the following steps:

[0038] In a three-neck flask equipped with a magnetic stirrer, a thermometer and a reflux condenser, the isotope13 The methyl iodide of C mark and chlorpromamine hydrochloride are added in the there-necked flask by molar ratio 2:1, then add the catalyst benzyltriethylammonium chloride of 1mol% (calculated as chlorpromamine hydrochloride) and concentration is 10wt % sodium hydroxide aqueous solution, wherein the molar ratio of sodium hydroxide to chlorpromamine hydrochloride is 3:1, the solvent is water, and react at normal pressure and 65°C for 12h; after the reaction is completed, cool to room temperature, and the reaction solution is After separation and purification, N,N-dimethylaminochloropropane is obtained; dry hydrogen chloride gas is passed into N,N-dimethylaminochloropropane, and stable ...

Embodiment 3

[0040] a stable isotope 13 C mark N, the synthetic method of N-dimethylaminochloropropane hydrochloride, the specific synthetic process of this method comprises the following steps:

[0041] In a three-necked flask equipped with a magnetic stirrer, a thermometer and a reflux condenser, the isotope 13 The iodomethane and chlorpromamine hydrochloride of C mark join in the there-necked flask by molar ratio 4:1, then add the catalyst benzyltriethylammonium chloride of 0.5mol% (calculated as chlorpropylamine hydrochloride) and concentration is 50wt% sodium carbonate toluene solution, wherein the molar ratio of sodium carbonate to chlorpropylamine hydrochloride is 8:1, the solvent is toluene, react at normal pressure and 95°C for 7h; after the reaction is completed, cool to room temperature, and the reaction solution is After separation and purification, N,N-dimethylaminochloropropane is obtained; dry hydrogen chloride gas is passed into N,N-dimethylaminochloropropane, and stable i...

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Abstract

The invention relates to a synthetic method for stable isotope labeled N,N-dimethylaminochloropropane hydrochloride. The method comprises the following steps: reacting stable isotope labeled iodomethane with chloropropylamine hydrochloride and an alkaline condensing agent under the action of a catalyst; carrying out separation and purification after completion of the reaction so as to obtain a stable isotope labeled N,N-dimethylaminochloropropane solution; introducing dry hydrogen chloride gas into the stable isotope labeled N,N-dimethylaminochloropropane solution; and carrying out separation and recrystallization so as to obtain stable isotope labeled N,N-dimethylaminochloropropane hydrochloride. Compared with the prior art, the method provided by the invention has the advantages of mild reaction conditions and simple and easily available reagents used in the method, and after separation and recrystallization, prepared N,N-dimethylaminochloropropane hydrochloride has chemical purity of more than 98.5% and isotopic abundance of more than 99 atom%.

Description

technical field [0001] The invention belongs to the field of stable isotope-labeled compounds, in particular to a synthesis method of stable isotope-labeled N,N-dimethylaminochloropropane hydrochloride. Background technique [0002] As a unique emerging material, stable isotopes and their labeled compounds have relatively low sensitivity and few available types, but compared with radioactive isotopes, they have the advantages of stable properties, easy operation, and no need for special protection. Since the 1970s, it has been widely used in analytical chemistry, pharmacology, organic chemistry, environment, nuclear power, electronics and other disciplines. [0003] Because mass spectrometry can provide both qualitative and quantitative information, developed countries require mass spectrometry to detect veterinary drug residues in food. At present, stable isotopes are the first choice for the detection of most contraband substances as internal standards (such as melamine, d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/15C07C209/00C07C209/08
Inventor 王伟杜晓宁罗勇卢伟京徐建飞张亮雷雯蔡银萍
Owner SHANGHAI RES INST OF CHEM IND
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