Unlock instant, AI-driven research and patent intelligence for your innovation.

Synthesis method of zolpidem tartrate

A technology of zolpidem tartrate and synthesis method, applied in chemical instruments and methods, carboxylate preparation, carboxylate preparation and other directions, can solve the problem of low yield and purity of zolpidem, low yield of zolpidem tartrate, etc. problem, to achieve the effect of improving yield and purity, and good effect

Pending Publication Date: 2022-02-18
ZHUZHOU QIANJIN PHARMA +1
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The yield and purity of zolpidem in the above-mentioned synthetic route are low, and there are various problems especially in the process of being applied to industrialized production, which further causes the yield of zolpidem tartrate to be lower

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Synthesis method of zolpidem tartrate
  • Synthesis method of zolpidem tartrate
  • Synthesis method of zolpidem tartrate

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0064] The preparation of intermediate 6 and zolpidem tartrate is also carried out by methods commonly used in the art.

[0065] The mass and volume in the mass-to-volume ratio of the present invention are standard units, such as the mass unit is g, the volume unit is ml, and the like.

Embodiment 1

[0068] This embodiment relates to the preparation of intermediate 1, comprising the following steps:

[0069] Preparation of Intermediate 1

[0070]

[0071] 200ml methylene dichloride is dropped into reaction flask, feeds dimethylamine gas, makes the dimethylamine reagent feed molar weight be 2 times of dichloroacetyl chloride, (the dimethylamine gas is made up of 40% dimethylamine solution Prepared by adding sodium hydroxide), controlling the reaction temperature at 0-5°C, and adding dropwise a dichloromethane solution (1 g / ml) containing 50.0 g of dichloroacetyl chloride.

[0072] After the reaction is complete, acid is added to adjust the pH to 7-8. Stir and stand for 20-30 minutes, separate the layers, and collect the organic layer. Drying under reduced pressure gave 47.85 g of intermediate 1 (N,N-dimethyl-2,2-dichloroacetamide). After testing, the yield was 92.1%, and the purity was 99.66%.

Embodiment 2

[0074] This embodiment relates to the preparation of intermediate 1, compared with embodiment 1, its difference is:

[0075] Using a dichloromethane solution (2 ml / g) containing 50.0 g of dichloroacetyl chloride, intermediate 1 was obtained with a yield of 90.4% and a purity of 98.36%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
purityaaaaaaaaaa
Login to View More

Abstract

The invention relates to a synthesis method of zolpidem tartrate. The synthesis method comprises the following steps: in the process of synthesizing an intermediate 1, firstly adding dichloromethane as a reaction solvent into a reactor, then introducing dimethylamine gas into the reactor, and finally, dropwise adding dichloroacetyl chloride into the reactor for a reaction, wherein in the process of synthesizing the intermediate 5, Pd-C / H2 is used as a reduction system. According to the invention, the overall synthesis route of zolpidem tartrate is optimized, and the yield and purity of zolpidem tartrate can be effectively improved. The method disclosed by the invention has a relatively good effect in industrial large-scale production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a method for synthesizing a zolpidem intermediate. Background technique [0002] Zolpidem tartrate is a white crystal, solid, stable to light and heat, soluble in water. Its trade names are Letan, Nuobin, Sinuosi, Zolpidem, its English name is Zolpidem Tartrate Tablets, and its chemical name is N, N, 6-trimethyl-2-(4-methylphenyl)-imidazo [1,2-a]pyridine-3-acetamide tartrate. The drug is a non-benzodiazepine short-acting imidazopyridine sedative-hypnotic developed by Sanofi, France, and is used to treat insomnia and brain diseases. Studies have shown that as a new generation of hypnotics, Zolpidem tartrate does not have a high affinity for the receptor GABA like traditional benzodiazepines, but it has high selectivity for the benzodiazepine receptor BZR1. The affinity is stronger than BZR2, and there is another special binding site, leading to the opening of chlorid...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/04C07C51/41C07C59/255
CPCC07D471/04C07C51/412C07C59/255Y02P20/55
Inventor 宿亮赵静芝金秉德钟超泽侯岳华郑席冬朱维君
Owner ZHUZHOU QIANJIN PHARMA