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A technology for zolpidem hydrochloride and a synthesis method, which is applied in the field of synthesis of intermediate zolpidem hydrochloride, can solve the problems of low purity, insufficient reaction, low product yield and the like, and achieves wide adaptability and good effect, yield and purity improvement
Pending Publication Date: 2022-02-18
ZHUZHOU QIANJIN PHARMA +1
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[0005] The above-mentioned N,N,6-trimethyl-2-(4-methylphenyl)-3-(2-chloro)dimethylaminocarbonylmethylimidazo[1,2-a]pyridine hydrochloride, The reaction in the process of preparing zolpidem hydrochloride by dechlorination is insufficient, the yield of the product is low, and the purity is low, which is not conducive to large-scale industrial production
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Embodiment 1
[0048] The present embodiment relates to a kind of preparation method of Zolpidem hydrochloride, comprises the following steps:
[0049] 1) 40g 2-chloro-N, N-dimethyl-2-(6-methyl-2-(p-tolyl) imidazo[1,2-a]pyridin-3-yl)acetamide hydrochloride Put the salt into the reactor, under the protection of nitrogen, add 200ml of methanol suspension containing 4.0g of Pd-C, pass in hydrogen, and react at 30-40°C for 2-3h;
[0050] 2) Cool to below 30°C, filter, distill part of the methanol from the filtrate, control the temperature at 0~-5°C, freeze and crystallize for 8-20h, filter, dry for 2-4h, add 100ml of acetone to reflux for 20-30min, cool down 0~- Cool and crystallize at 5°C for 8-20h. Filter and wash with a small amount of acetone to obtain white solid crystals, dry at 40-60°C for 4 hours to obtain 26.57g of Zolpidem hydrochloride, the yield is 73.07%, the purity is 99.95%, ESI: m / z [M+H ] + 344.18. The resulting product was analyzed by liquid chromatography, and its chromato...
Embodiment 2
[0052] This embodiment relates to a preparation method of Zolpidem hydrochloride, compared with Example 1, the difference is:
[0053] Amplify 2-chloro-N,N-dimethyl-2-(6-methyl-2-(p-tolyl)imidazo[1,2-a]pyridin-3-yl)acetamide hydrochloride to 1.0Kg, the yield is 78.93%, and the purity is 98.39%.
Embodiment 3
[0055] This example relates to a preparation method of Zolpidem hydrochloride. Compared with Example 1, the difference is that methanol is replaced by isopropanol, the yield is 72.35%, and the purity is 95.04%.
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Abstract
The invention belongs to the technical field of chemical synthesis, and particularly relates to a synthesis method of zolpidem hydrochloride. According to the method disclosed by the invention, in the process of preparing zolpidem hydrochloride from 2-chloro-N,N-dimethyl-2-(6-methyl-2-(p-tolyl)imidazo[1,2-a]pyridin-3-yl)acetamide hydrochloride, Pd-C/H2 is selected as a reduction system. According to the method disclosed by the invention, the yield and the purity of zolpidem hydrochloride can be effectively improved, wherein the yield is improved from original 20% or so to about 70% and the purity is improved from original 60% or so to about 99%. The yield and purity of the method disclosed by the invention in an industrial amplification experiment are even superior to yield and purity obtain in small-scale reaction in a laboratory, so the method disclosed by the invention is particularly suitable for large-scale industrial production.
Description
technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a method for synthesizing zolpidem hydrochloride, an intermediate of zolpidem tartrate. Background technique [0002] Zolpidem (Ⅰ), the English name is Zolpidem, the chemical name is N,N,6-trimethyl-2-(4-methylphenyl)-imidazo[l,2-a]pyridine-3-ethane Amide is a non-benzodiazepine imidazopyridine short-acting sedative-hypnotic drug developed by Sanofi, France. It was first launched in 1988 for the treatment of insomnia and brain diseases. Clinical studies have shown that zolpidem, as a new generation of hypnotics, has high selectivity for the benzodiazepine receptor BZR l has a stronger affinity than BZR 2 , the half-life is short, the duration of action is only 1.6 hours, there is no rebound after drug withdrawal, the side effects are small, and there is no inhibitory effect on breathing. It is one of the most popular sedative-hypnotics at present. Currently, there a...
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