Deuterated diazepam and preparation method thereof

Abstract

The invention discloses deuterated diazepam and a preparation method thereof. The preparation method of deuterated diazepam comprises the following steps of: (1) mixing 7-chlorine-1-methyl-5-phenyl-1,3-dihydro-1,4-benzodiazepine-2-ketone and N,N-dimethyl formamide, and stirring; (2) adding potassium carbonate and deuterated chloroform, heating the mixture to more than 40 DEG C and stirring; and (3) carrying out separation to obtain the deuterated diazepam. The preparation method provided by the invention is short, simple and convenient to operate, low in cost and easy to purify. The commercially available non-deuterated diazepam uses a small amount of deuterated reagents as deuterium sources in a non-deuterated solvent atmosphere, so that deuterated diazepam is obtained in a relatively short period of time, and through simple column chromatography purification, a purified product is purified. The deuterated diazepam standard product prepared according to the invention is high in purity and stable in chemical property; and the preparation of the standard product for analysis is convenient. The preparation method provided by the invention can be used for producing deuterated internal standard substance used for analyzing and detecting diazepam.

Description

technical field [0001] The invention relates to the field of chemical analysis and detection, in particular to a deuterated diazepam standard product and a preparation method thereof. Background technique [0002] Diazepam is a benzodiazepine central nervous system depressant, which can cause inhibition of different parts of the central nervous system. As the dosage increases, the clinical manifestations can range from mild sedation to hypnosis or even coma. In recent years, criminal cases such as poisoning, suicide, and misuse caused by such drugs have occurred from time to time. This requires the public security judicial appraisal department to test the samples of samples involving such drugs. The means to ensure that the detection method is accurate and reliable is to add an internal standard during detection, and deuterium is the best internal standard. Because its use is non-civilian, it has particularity. For this reason, in our country, for this kind of standard Ther...

AI Technical Summary

Problems solved by technology

The means to ensure that the detection method is accurate and reliable is to add an internal standard during detection, and deuterium is the best internal standard. Because its use is non-civilian, it has particularity. For this reason, in our country, for this kind of standard There are relatively few researches and productions, and such standard products are necessary and indispensable in analysis and detection. For a long time, the deuterated internal standards used in my country have been dependent on imports. The wide use of such standard products in China

[0003] The method reported in the literature selects deuterated sodium hydroxide and expensive deuterated methanol as the deuterium source and reaction medium that are easy to absorb water and deteriorate, and even selects a very strong organic base of potassium tert-butoxide. This method has harsh conditions and relatively low cost. Expensive, cumbersome operation and other disadvantages

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