The synthetic technique of meclofenoxate hydrochloride crude product

A technology of meclofenoxate hydrochloride and synthesis process, which is applied in the preparation of organic compounds, preparation of aminohydroxyl compounds, organic chemistry, etc., can solve the problems such as the unreported synthesis method of crude meclofenoxate hydrochloride, and achieve the reduction of production cost Effect

Active Publication Date: 2015-10-28
JIANGSU HI STONE PHARMA
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Problems solved by technology

[0005] In the production process of meclofenoxate hydrochloride, it is necessary to synthesize the crude product of meclofenoxate hydrochloride earlier, and then refine and make the meclofenoxil hydrochloride of finished product. However, in the prior art, methyl chloride hydrochloride of high quality and high yield The synthetic method of fen ester crude product has not yet been reported

Method used

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  • The synthetic technique of meclofenoxate hydrochloride crude product
  • The synthetic technique of meclofenoxate hydrochloride crude product

Examples

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Comparison scheme
Effect test

Embodiment

[0028] Example: Synthesis of crude meclofen axetil hydrochloride (calculated in batch 47kg).

[0029] (10) Before starting production, check that the equipment and workplace have no products, documents or materials unrelated to the production of this batch of products left over from the previous batch, and the equipment is in a clean and ready-to-use state; Valves, measuring instruments, monitoring instruments and auxiliary equipment are in good condition;

[0030] (20) synthesis reaction, its concrete steps include: heating to reflux, cooling, reflux decolorization, suction filtration and standing for stratification;

[0031] (21) heating to reflux: open the vacuum of the reaction tank, pump 181kg of toluene into the first reaction tank of 500L, open stirring, pump 24.7kg of dimethylaminoethanol, open the feeding port of the first reaction tank, drop into p-chlorophenoxyacetic acid 39.5kg, 1.2kg of p-toluenesulfonic acid, open the first reaction tank jacket steam, stir to be...

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Abstract

The invention discloses a synthetic process of crude meclofenoxate hydrochloride. The synthetic process comprises the following steps: checking and cleaning a detection instrument, production equipment and a working place before production, performing a heating reflux reaction on toluene, tolueneaminoethanol, p-chlorophenoxyacetic acid and toluenesulfonic acid, cooling, decolorizing, performing suction filtration on decolorizing liquid, standing and layering filter liquor, performing suction filtration, immersion cleaning and vacuum drying on upper-layer crystals to prepare crude meclofenoxate hydrochloride, and finally weighing and packaging. According to the synthetic process, high-quality crude meclofenoxate hydrochloride can be prepared, the yield is 74.0%-78.0%, a good foundation is laid for refining meclofenoxate hydrochloride, and the production cost is reduced.

Description

technical field [0001] The invention relates to the field of drug synthesis, in particular to a synthesis process of a crude meclofen axetil hydrochloride. Background technique [0002] Meclofenoxate Hydrochloride, the chemical name of this product is 2-(dimethylamino)ethyl-p-chlorophenoxyacetate hydrochloride, and its structural formula is [0003] , calculated as dry product, containing C 12 H 16 ClNO 3 ·HCl should not be less than 98.6%. This product is a white crystalline powder; it has a slightly specific smell, sour and bitter taste, easily soluble in water, soluble in chloroform, and almost insoluble in ether. [0004] Meclofen axetil hydrochloride can promote the redox process of cells, increase the utilization of carbohydrates, and regulate the metabolism of nerve cells. One of the central stimulants. [0005] In the production process of meclofen axetil hydrochloride, it is necessary to synthesize the crude product of meclofen axetil hydrochloride first, an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C219/06C07C213/06C07C213/08
Inventor 王多平
Owner JIANGSU HI STONE PHARMA
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