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Preparation method of 1-carboxyalkyl diazepam

A technology based on diazepam, which is applied in the field of preparation of 1-carboxyalkyl diazepam, can solve the problems of time-consuming, expensive equipment, troublesome sample processing, etc., and achieve the effect of high purity and simple and effective synthesis steps

Inactive Publication Date: 2015-01-07
JIANGNAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the detection of diazepam at home and abroad mainly includes high-performance liquid chromatography (HPLC), gas chromatography (GC), thin-layer chromatography (TLC), gas-mass spectrometry (GC-MS), liquid-mass Combined method (LC-MS), etc., although the detection is accurate, the equipment is expensive and requires professionals, and the sample pretreatment is cumbersome and time-consuming

Method used

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  • Preparation method of 1-carboxyalkyl diazepam
  • Preparation method of 1-carboxyalkyl diazepam
  • Preparation method of 1-carboxyalkyl diazepam

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Embodiment 1

[0020] (1) Preparation of methyl 6-bromohexanoate (b): Add 1.95 g of 6-bromohexanoic acid (10 mmol) into 10 mL of methanol, slowly add thionyl chloride (15 mmol) dropwise under stirring in an ice bath, and then raise the temperature To reflux, keep reflux at 50°C for 2-3h. After the reaction was completed, vacuum rotary evaporation at 45°C was performed to spin dry, and then methanol was added to spin dry and repeated twice (10 mL×2) to obtain the substance 6-bromohexanoic acid methyl ester (b) for future use.

[0021] (2) Synthesis of 1-methylhexanoate diazepam (c): Dissolve norazepam (substance a, 1.682g, 6.213mmol) and 18-crown-6 (1.64g, 6.213mmol) in 100mL Add sodium methoxide solution (12.4 mL, 6.213 mmol) to water in tetrahydrofuran under cooling in an ice bath and stir, stir at room temperature for 1 h, and set aside.

[0022] Under ice cooling, methyl 6-bromohexanoate (1.3 g, 6.213 mmol) was added dropwise to the above solution, stirred at room temperature for 12 h, t...

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Abstract

The invention provides a preparation method of 1-carboxyalkyl diazepam, and belongs to the technical field of biochemical engineering. According to the preparation method, nordazepam and 18-crown ether-6 are mixed in the molar ratio of 1:1 and cooled in ice bath, and a sodium methoxide solution with equal molar weight is added for reaction at the room temperature for standby; under ice-bath cooling, 6-methyl bromohexanoate with equal molar weight is added, is stirred at the room temperature, and stays overnight to prepare esterified ester; the esterified ester is dissolved in a tetrahydrofuran-pure water solution for reaction at the room temperature and stays overnight, and then purification is performed to obtain a product 1-carboxyalkyl diazepam. The preparation method is simple and effective in synthesis step, the purity of the product is very high via identification, and requirements for domestic immune research on diazepam medicine can be met.

Description

technical field [0001] The invention relates to a preparation method of 1-carboxyalkyl diazepam, which belongs to the technical field of biochemical industry. Background technique [0002] Diazepam, also known as stability, is a benzodiazepine sedative and hypnotics, belonging to the second generation of hypnotic sedatives, chemical name: 1-methyl-5-phenyl-7-chloro-1,3-di Hydrogen-2H-1,4-benzodiazepine-2-one. However, some breeding enterprises use it as an animal feed additive in order to increase feed remuneration, causing animals to be sleepy and less active, grow faster and have the effect of changing meat quality. It is also useful for sedation before animal slaughter, quarantine, or animal transfer, transportation, and slaughter, so as to relieve animal tension and reduce animal injury and mortality. Drowsiness, weakness, headache, dizziness, nausea, constipation, and occasional rash, liver damage, bone marrow suppression and other adverse reactions can be seen with t...

Claims

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Application Information

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IPC IPC(8): C07D243/26
CPCC07D243/26
Inventor 徐丽广官丹丹胥传来匡华马伟刘丽强宋珊珊吴晓玲
Owner JIANGNAN UNIV
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