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Synthetic process of crude meclofenoxate hydrochloride

A technology of meclofenxate hydrochloride and synthesis process, applied in the preparation of organic compounds, preparation of aminohydroxy compounds, organic chemistry, etc., can solve problems such as unreported synthetic method of crude meclofenxate hydrochloride, and reduce production costs Effect

Active Publication Date: 2014-10-01
JIANGSU HI STONE PHARMA
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  • Abstract
  • Description
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Problems solved by technology

[0006] 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 reported

Method used

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  • Synthetic process of crude meclofenoxate hydrochloride
  • Synthetic process of crude meclofenoxate hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0029] Embodiment: the synthesis of the crude product of meclofenoxate hydrochloride (based on a batch size of 47kg).

[0030] (10) Before production starts, check that there are no products, documents or materials unrelated to the production of this batch of products left over from the previous batch in the workplace, and the equipment is in a clean and ready-to-use state; Valves, measuring instruments, monitoring instruments and auxiliary instruments are in good condition;

[0031] (20) Synthetic reaction, the specific steps of which include: heating to reflux, cooling, reflux for decolorization, suction filtration and static stratification;

[0032] (21) Heating and reflux: Turn on the vacuum of the reaction tank, pump 181kg of toluene into the 500L first reaction tank, start stirring, pump in 24.7kg of dimethylaminoethanol, open the feeding port of the first reaction tank, and put in p-chlorophenoxyacetic acid 39.5kg, 1.2kg of p-toluenesulfonic acid, turn on the jacket st...

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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

[0001] technical field [0002] The invention relates to the field of drug synthesis, in particular to a synthesis process of crude meclofenoxate hydrochloride. Background technique [0003] Meclofenoxate Hydrochloride, the chemical name of this product is 2-(dimethylamino)ethyl p-chlorophenoxy acetate hydrochloride, and its structural formula is [0004] , calculated as dry product, including C 12 h 16 ClNO 3 · HCl must not be less than 98.6%. This product is a white crystalline powder; slightly specific smell, bitter taste, easily soluble in water, soluble in chloroform, almost insoluble in ether. [0005] Meclofenoxate hydrochloride can promote the oxidation-reduction process of cells, enhance the utilization of carbohydrates, and regulate the metabolism of nerve cells. It is widely used in the treatment of coma, traumatic brain injury, disturbance of consciousness caused by stroke, Alzheimer's disease, and mental retardation in children. One of the central stimula...

Claims

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Application Information

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IPC IPC(8): C07C219/06C07C213/06C07C213/08
Inventor 王多平
Owner JIANGSU HI STONE PHARMA
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