Preparation method of Pramiracetam sulfate

A technology for pramiracetam sulfate and chloroethylamine hydrochloride, which is applied in the field of preparation of pharmaceutical compounds, can solve the problems of many by-products, increase one-step reaction, and high temperature, achieve easy availability, improve environmental friendliness, and reduce emissions Effect

Active Publication Date: 2015-02-11
北京华睿鼎信科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantage is that it needs to prepare 2-pyrrolidone sodium salt with strong base sodium methylate, which increases one-step reaction
Its disadvantage is that in the preparation process, the phase transfer catalyst TEBA is used, the temperature is too high during the reaction process, and there are too many by-products

Method used

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  • Preparation method of Pramiracetam sulfate
  • Preparation method of Pramiracetam sulfate
  • Preparation method of Pramiracetam sulfate

Examples

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Embodiment 1

[0044] (1) Preparation of N,N-diisopropyl-2-chloroethylamine hydrochloride

[0045] Add 40.95kg of thionyl chloride into a 100L reaction kettle, stir mechanically, cool in an ice-salt bath, and drop the temperature in the reaction kettle to 0-5°C, slowly add 25.00kg of N,N-diisopropylethanolamine dropwise, After the addition, the temperature was raised to 75-80° C. to continue the reaction for 10 h, and the reaction was detected by TLC (developing solvent: dichloromethane: methanol: ammonia water = 20:4:1, iodine color development). When the inner temperature of the reaction kettle drops to 30-40°C, slowly add 5.52 kg of methanol under the condition of mechanical stirring. Then the temperature was controlled at 55-60°C, and distillation was performed under reduced pressure to obtain a reddish-brown solid; 22.00 kg of ethanol / isopropyl ether (1:10) mixed solvent was added, stirred and crystallized at 0-5°C for 10 hours, and dried with a centrifuge to obtain Pale yellow solid w...

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Abstract

The invention relates to a preparation method of Pramiracetam sulfate. The preparation method comprises the steps of using N, N-diisopropylethanolamine as a starting raw material, and conducting chlorination and ammonolysis to obtain an intermediate N, N- diisopropylethylene diamine; then conducting acylation, substitution, salt forming and refining to obtain the Pramiracetam sulfate. The preparation method of the Pramiracetam sulfate has the characteristics that the reaction process is safe and controllable, the cost of used raw materials and solvent is low and the raw materials and the solvent are easy to obtain; organic solvent is very easy to recycle, the emission of organic matters is greatly reduced, and the environmental friendliness is improved; since the intermediate N-[(2-diisopropyl amino) ethyl]-chloroacetamide is not separated and purified, the reaction equipment is simplified, and the operation process is enabled to be more high-efficient.

Description

technical field [0001] The invention relates to the preparation of pharmaceutical compounds, in particular to a preparation method of pramiracetam sulfate. Background technique [0002] Pramiracetam sulfate has the following structural formula: [0003] [0004] It was developed by the Warner-Lambert Company of the United States. It was first launched in Italy in 1993, and has been listed in Argentina, Australia, France, Japan and other countries successively. At present, my country does not import the raw materials and preparations of this product. [0005] Pramiracetam belongs to the class of pyrrolidone nootropics. It is a high-efficiency, low-toxicity, and well-tolerated cognitive activator. It is a cyclic derivative of γ-aminobutyric acid. It can promote the conversion of ADP into ATP in the brain, promote the synthesis of acetylcholine and enhance the conduction of nerve excitement. It has a strong ability to improve brain function, enhance memory, and promote brai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/27
CPCC07D207/27
Inventor 安明祝江业
Owner 北京华睿鼎信科技有限公司
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