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Method for preparing medical compound chlorphenesin

A technology of chlorphenesin and compounds, which is applied in the field of preparation of the pharmaceutical compound chlorphenesin, can solve problems such as troublesome operation of solvent recovery, difficult safety control, and strong anesthesia, and achieve equipment saving, low raw material prices, and anesthesia strong effect

Inactive Publication Date: 2012-05-02
天津市美索药物研发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] 1. The boiling point (bp) of the mixed solvent diethyl ether-petroleum ether is 34.5°C, which is highly volatile, flammable, and highly narcotic, so it has high requirements for workshop equipment and environment, and it is difficult to control the safety in production, and the recovery of solvent operation is also difficult trouble

Method used

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  • Method for preparing medical compound chlorphenesin
  • Method for preparing medical compound chlorphenesin
  • Method for preparing medical compound chlorphenesin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Put epichlorohydrin (100g) into the reaction bottle, stir, put in 200ml dilute sulfuric acid, heat to 100-105°C, reflux for 1 hour, cool down to 80°C, add p-chlorophenol (128.6g) and 37% hydrogen Sodium oxide aqueous solution, heated to 105-115°C, alkaline reflux reaction for 1 hour; cooled to 75°C, added appropriate amount of dilute hydrochloric acid for neutralization, controlled pH 5.5-6.5, poured into a separatory funnel, stood still, separated, the lower layer The oil was crystallized in stirred chloroform, frozen for 4 hours, suction filtered, dried at 40-45°C for 2 hours, and dried at 60°C for 6 hours, with a melting point of 77°C to obtain 182 grams of chlorophenesin. The method for recovering chloroform: washing with water 1 to 2 times, let stand, separate layers, collect the chloroform layer, which can be recycled.

Embodiment 2

[0027] Put epichlorohydrin (100g) into the reaction flask, stir, add dilute sulfuric acid 200ml, heat, reflux for 1 hour, cool down to 80°C, add p-chlorophenol (128.6g) and 37% aqueous sodium hydroxide solution, heat , alkaline reflux reaction for 1 hour; lower the temperature to 75°C, add an appropriate amount of dilute hydrochloric acid to neutralize, control the pH to 5.5-6.5, pour it into a separatory funnel, let it stand, separate layers, and put the lower layer of oil into the stirred ethanol-water solution for analysis. crystallization, freezing for 8 hours, suction filtration, and drying of the filter cake (it is advisable to gradually increase the drying temperature in stages), with a melting point of 77±2°C to obtain 183g of the product.

[0028] Refining method: use ethanol-water (2:8 or 3:7) 2 to 6 times as the refining solvent, put in crude ethanol-water and activated carbon, heat and reflux for 30-45 minutes, heat filter, the filtrate is cooled to room temperature...

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Abstract

The invention belongs to the organic chemical field and relates to a method for preparing a medical compound chlorphenesin; wherein, the chlorphenesin belongs to an antifungal drug. For more than ten years, the product is internationally applied in necessities, such as medical soaps, soaps, ointments, nail polishes, etc. The product is also an intermediate product for preparing chlorphenesin carbamate. The invention has the advantages of easy preparation method and technique operation, easy industrialized production, high safety and stable product quality.

Description

technical field [0001] The invention belongs to the field of organic chemistry and relates to a preparation method of a medicinal compound chlorphenesin. Background technique [0002] Chlorphenesin is an antifungal drug, which is suitable for antifungal, bacterial, vaginal mold, and trichomonas diseases. There are many dosage forms of medicines. Over the past ten years, chlorphenesin has been used in the manufacture of pharmaceutical toothpaste, nail polish, soap, soap and other daily products abroad; this product is also an intermediate for the preparation of chlorphenesin carbamate. Retrieval of foreign literature, British patent GB628497 reports: adopt p-chlorophenol and glycidol to react in the presence of pyridine, and post-treatment with chloroform or ether-petroleum ether to obtain the product chlorophenesin. [0003] Reaction formula: [0004] [0005] Operation method: [0006] p-Chlorophenol (12.8g) and glycidol (7.4g), heated and refluxed until it was a clea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/23C07C41/03
Inventor 张志毅王若王围
Owner 天津市美索药物研发有限公司
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