Method for preparing 3-(N-methyl-N-pentyl amido) propionate alkoxide

A technology of propionate hydrochloride and amylamino, applied in the field of preparation of 3-propionate hydrochloride, can solve problems such as toxicity, safety hazards, product loss, etc.

Active Publication Date: 2009-10-07
CHENGDA PHARM CO LTD
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, because acrylonitrile is not only toxic in vapor, but also easily poisoned through the skin when attached to the skin, there are certain safety hazards in industrial production, and the recrystallization of butanone will also cause certain losses to the product.

Method used

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  • Method for preparing 3-(N-methyl-N-pentyl amido) propionate alkoxide
  • Method for preparing 3-(N-methyl-N-pentyl amido) propionate alkoxide

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Embodiment Construction

[0011] The present invention will be further described below by way of examples.

[0012] The preparation method of 3-(N-methyl-N-pentylamino) propionate hydrochloride comprises the following steps successively:

[0013] A. Amylamine and benzaldehyde with a molar ratio of 1.05-1.3:1 are dehydrated in the presence of toluene or benzene at a reaction temperature of 110-130° C. and a reaction time of 1-2 hours. After the dehydration is completed, slowly add dimethyl sulfate with a molar ratio of 1 to 1.3:1 to pentylamine dropwise. React for a period of time under heating, add water after cooling, and separate layers; take the water layer, add NaOH with a molar ratio of 2 to 3:1 to pentylamine, and KOH or NaOH can also be used. 2 CO 3 or K 2 CO 3 , Separate the amine layer; take the amine layer and undergo a distillation at 90-95°C to obtain N-methylpentylamine.

[0014] B. Mix N-methylpentylamine, 3-halopropionate and alkali in a solvent, and stir under heating until the rea...

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Abstract

The method discloses a preparation method of 3-(N-methyl-N-pentylamino) propionate hydrochloride, and aims to provide a method with high yield, simple operation, low moisture absorption, high safety performance and low loss Small and other advantages, suitable for large-scale industrial production of 3-(N-methyl-N-pentylamino) propionate hydrochloride preparation method. It includes pentylamine, benzaldehyde, dimethyl sulfate and alkali as raw materials, which are synthesized into N-methylpentylamine through dehydration, addition and distillation; N-methylamylamine, 3-halogenated propionate and Alkali as raw material, synthesize 3-(N-methyl-N-pentylamino) propionate in a solvent; use 3-(N-methyl-N-pentylamino) propionate as raw material, obtain by hydrolysis and acidification 3-(N-Methyl-N-pentylamino)propion hydrochloride. The product of the invention is a drug intermediate for synthesizing sodium ibandronate.

Description

technical field [0001] The present invention relates to the preparation method of medicine intermediate, especially the preparation method of 3-(N-methyl-N-pentylamino)propion hydrochloride. Background technique [0002] 3-(N-methyl-N-pentylamino) propionate hydrochloride is an intermediate in the synthesis of ibandronate sodium (Ibandronate Monosodium), and ibandronate sodium belongs to the third generation of bisphosphonate drugs, is An anti-hypercalcemia drug with high efficiency and low toxicity has gradually become the drug of choice for the treatment of hypercalcemia complicated by malignant tumors and bone pain caused by osteolytic cancer metastasis. With the aging of the world's population, senile osteoporosis is a common disease of the elderly, and foreign countries are clinically studying the use of ibandronate sodium to supplement calcium. The market prospect of 3-(N-methyl-N-pentylamino) propionate hydrochloride is promising. Its chemical structural formula is:...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C227/18C07C227/04C07C229/12
Inventor 葛建利文春林
Owner CHENGDA PHARM CO LTD
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