Deuterated estazolam and preparation method thereof

Abstract

The invention discloses deuterated estazolam and a preparation method thereof. The preparation method comprises following steps of (1) adding 6-phenyl-8-chlorine-4H-[1,2,4] triazole-[4,3-a][1,4] benzo-diazepine into dimethyl sulfoxide or N,N-dimethylformamide, mixing and stirring; (2) adding a catalyst cesium carbonate or potassium carbonate as well as deuterated chloroform, stirring and heating up to over 40DEG C; and (3) separating so as to obtain deuterated estazolam. The preparation method is concise, is simple and convenient to operate, has low cost, and is easy for purification. Commercially available non-deuterated estazolam can be converted into deuterated estazolam by a little deuterated reagent used as a deuterium source in the non-deuterated solvent atmosphere in shorter time, and a pure product can be obtained through simple purification by column chromatography. The standard deuterated estazolam prepared by the method has high purity and stable chemical property, and is convenient for preparing standard substances for analysis. The preparation method can be used for producing, analyzing and detecting the deuterated internal standard substance used by estazolam.

Description

technical field [0001] The invention relates to the field of chemical analysis and detection, in particular to a deuterated estazolam standard product and a preparation method thereof. Background technique [0002] Estazolam 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 Th...

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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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