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Deuterated alprazolam and preparation method thereof

A technology of deuterated alprazolam and alprazolam, which is applied in the field of deuterated alprazolam standard product and its preparation, can solve the problems such as restricted wide use, high price, etc., and achieves convenient operation, low cost, and easy preparation. method short effect

Inactive Publication Date: 2015-04-15
INST OF FORENSIC SCI OF MIN OF PUBLIC SECURITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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
At present, no literature has been retrieved to report the synthesis of this type of compound

Method used

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  • Deuterated alprazolam and preparation method thereof
  • Deuterated alprazolam and preparation method thereof
  • Deuterated alprazolam and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a 100mL three-necked flask with a reflux condenser, put a stirring bar, stir with a magnetic force, then add 154mg, 0.5mmol non-deuterated alprazolam into the three-necked flask, and then add 10mL N, N-dimethylformamide , stirred at room temperature for 30 minutes to fully dissolve it, then added 138 mg of powdered potassium carbonate and 1 milliliter of deuterated chloroform in the three-necked flask, and replaced the three-necked flask with nitrogen three times at this time to remove air and moisture in the three-necked flask, and then placed the three-necked flask In an oil bath, raise the temperature to 120 degrees Celsius, stir and react for 2 hours, turn off the oil bath, place the reaction flask at room temperature to cool, and after cooling to room temperature, add 20 ml of water to the three-necked flask. At this time, the mixed liquid in the three-necked flask Transfer to a 100mL separatory funnel, and add 20mL of ethyl acetate to the separatory funnel. Afte...

Embodiment 2

[0030] Embodiment 2 (comparative example)

[0031]In a 100mL three-necked flask with a reflux condenser, put a stirring bar, stir with magnetic force, then add non-deuterated alprazolam (154mg, 0.5mmol) into the three-necked flask, and then add 10mL N, N-dimethyl Dimethyl formamide, stirred at room temperature for 30 minutes to make it fully dissolved, then added 138 mg of powdered potassium carbonate and 1 milliliter of deuterated chloroform in the three-necked flask, and now the three-necked flask was replaced with nitrogen three times to remove air and moisture in the three-necked flask, and then After the three-necked flask was stirred at room temperature for 24 hours, 20 ml of water was added to the three-necked flask. At this time, the mixed solution in the three-necked flask was transferred to a 100 mL separating funnel, and 20 mL of ethyl acetate was added to the separating funnel, and the mixture was shaken fully. After uniformity, let stand to separate the layers, se...

Embodiment 3

[0033] In a 100mL three-necked flask with a reflux condenser, put a stirring bar, stir with magnetic force, then add non-deuterated alprazolam (154mg, 0.5mmol) into the three-necked flask, and then add 10mL N, N-dimethyl Dimethyl formamide, stirred at room temperature for 30 minutes to make it fully dissolved, then added 138 mg of powdered potassium carbonate and 0.5 milliliters of deuterated chloroform in the three-necked flask, and now the three-necked flask was replaced with nitrogen three times to remove air and moisture in the three-necked flask, and then The three-necked flask was placed in an oil bath, heated to 120 degrees Celsius, stirred and reacted for 6 hours, the oil bath was closed, and 20 milliliters of water was added to the three-necked flask. Add 20mL of ethyl acetate to the separatory funnel, shake it well, let stand to separate the layers, separate the ethyl acetate layer, continue to shake the water layer with 20mL of ethyl acetate to shake and extract, and...

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Abstract

The invention discloses deuterated alprazolam and a preparation method thereof. The preparation method of deuterated alprazolam comprises the following steps of: (1) mixing commercially available non-deuterated alprazolam 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 alprazolam. 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 alprazolam uses a small amount of deuterated reagents as deuterium sources in a non-deuterated solvent atmosphere, so that deuterated alprazolam is obtained in a relatively short period of time, and through simple column chromatography purification, a purified product is purified. The deuterated alprazolam 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 alprazolam.

Description

technical field [0001] The invention relates to the field of chemical analysis and detection, in particular to a deuterated alprazolam standard product and a preparation method thereof. Background technique [0002] Alprazolam is a benzodiazepine central nervous system depressant, which can cause inhibition of different parts of the central nervous system. With the increase of dosage, 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 stand...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/04
Inventor 杜鸿雁张蕾萍董颖王瑞花栾玉静常靖于忠山何毅王芳琳王炯张云峰侯小平崔冠峰
Owner INST OF FORENSIC SCI OF MIN OF PUBLIC SECURITY
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