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Dioxopromethazine hydrochloride and preparation method thereof

A technology of dioxypromazine hydrochloride and dioxypromazine, which is applied in directions such as organic chemistry and chemical recovery, can solve the problems of long reaction time, increased production cost, loss of activity, etc. simple effect

Active Publication Date: 2020-11-17
上海金不换兰考制药有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This preparation method adopts palladium acetate as catalyzer, and price is more expensive, is difficult for recycling, has improved production cost, and easily occurs palladium poisoning, thereby makes palladium acetate lose activity, affects the effect of oxidation, adopts oxygen as oxidant in addition, and reaction time is shorter long, increasing the cost of the equipment

Method used

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  • Dioxopromethazine hydrochloride and preparation method thereof
  • Dioxopromethazine hydrochloride and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0024] A preparation method for dioxpromazine hydrochloride, comprising the following steps:

[0025] (1) Oxidation reaction: Cool solution A to 10°C, slowly add potassium persulfate solution, keep warm for 25 minutes after adding, heat to 30°C, keep warm for 5 hours, oxidize promethazine to dioxpromethazine, and obtain a solution B, Potassium persulfate solution was prepared by using 45.74g of potassium persulfate and 160mL of purified water.

[0026] Solution A was prepared as follows:

[0027] 1) join in the flask in the promethazine hydrochloride of 20g, add the purified water of 80ml and the hexanaphthene of 80ml, stir well, then under the condition of 30 ℃, add dropwise the aqueous solution of 15wt% sodium hydroxide, adjust the mixed solution The pH was 10, stirred for 20 min, allowed to stand for stratification, and the organic phase was separated, and the organic phase was washed twice with purified water;

[0028] 2) Place the washed organic phase (promethazine cycl...

Embodiment 2

[0038] A preparation method for dioxpromazine hydrochloride, comprising the following steps:

[0039] (1) Oxidation reaction: Cool solution A to 0°C, slowly add potassium hydrogen persulfate solution, keep warm for 15 minutes after adding, heat to 10°C, keep warm for 4 hours, oxidize promethazine to dioxpromethazine, and obtain a solution B, Potassium persulfate solution was prepared by using 40g of potassium persulfate and 160mL of purified water.

[0040] Solution A was prepared as follows:

[0041] 1) join in the flask in the promethazine hydrochloride of 15g, add the purified water of 70ml and the hexanaphthene of 70ml, stir well, then under 10 ℃ of conditions, add dropwise the aqueous solution of 15wt% sodium hydroxide, adjust the mixing solution The pH was 9, stirred for 10 minutes, allowed to stand and separated, and the organic phase was separated, and the organic phase was washed twice with purified water;

[0042] 2) Place the washed organic phase (promethazine cyc...

Embodiment 3

[0048] A preparation method for dioxpromazine hydrochloride, comprising the following steps:

[0049] (1) Oxidation reaction: Cool solution A to 5°C, slowly add potassium hydrogen persulfate solution, keep warm for 35 minutes after adding, heat to 20°C, keep warm for 4.5h, oxidize promethazine to dioxpromethazine, and obtain Solution B, potassium persulfate solution was prepared by using 45g of potassium persulfate and 160mL of purified water.

[0050] Solution A was prepared as follows:

[0051] 1) join in the flask in the promethazine hydrochloride of 25g, add the purified water of 80ml and the hexanaphthene of 80ml, stir, then dropwise the sodium hydroxide solution of 15wt% under the condition of 20 ℃, adjust the mixed solution The pH was 12, stirred for 30 minutes, allowed to stand for stratification, and the organic phase was separated, and the organic phase was washed twice with purified water;

[0052] 2) Place the washed organic phase (promethazine cyclohexane soluti...

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Abstract

The invention provides dioxopromethazine hydrochloride and a preparation method thereof. The preparation method comprises the following steps: (1) oxidation reaction: preparing a solution A containingfree isopromethazine, dropwise adding a potassium hydrogen persulfate solution into the solution A under the low-temperature condition to oxidize the isopromethazine into dioxopromethazine to preparea solution B; (2) salifying reaction: dissociating the dioxopromethazine in the solution B into dichloromethane by using sodium hydroxide, washing an organic phase by using water, removing a solvent,dissolving the organic phase after the solvent is removed by using acetone, and introducing hydrogen chloride gas into the acetone to prepare a dioxopromethazine hydrochloride crude product; and (3)refining reaction: dissociating the dioxopromethazine hydrochloride crude product into a dioxopromethazine basic group by using sodium hydroxide, dissolving in acetone, decolorizing by using activatedcarbon, carrying out suction filtration, and introducing hydrogen chloride gas into acetone to prepare a dioxopromethazine hydrochloride refined product. According to the process, hydrogen persulfateis adopted as an oxidizing agent, so that operation is easy and safe, the requirement for equipment is not high, pressurization is not needed, energy consumption is low, the yield of dioxopromethazine hydrochloride is high, and the purity is high.

Description

technical field [0001] The invention relates to the technical field of organic synthesis of dioxamethazine hydrochloride, in particular to a dioxamethazine hydrochloride and a preparation method thereof. Background technique [0002] Dioxetazine hydrochloride has a strong antitussive effect, and has antihistamine, smooth muscle spasm relief, anti-inflammatory and local anesthetic effects. The existing dioxpromazine hydrochloride preparation methods mostly use the hydrogen peroxide oxidation system, which requires heating or reflux, which is a dangerous chemical process with high safety risks, high requirements for equipment, and complicated preparation steps. [0003] CN106749098B discloses a method for preparing dioxpromethazine hydrochloride with oxygen as an oxidizing agent. The raw material promethazine hydrochloride is used as a substrate, and after alkaline hydrolysis, promethazine is obtained. Oxygen is used as an oxidizing agent and palladium acetate is used as a cat...

Claims

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Application Information

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IPC IPC(8): C07D279/34
CPCC07D279/34Y02P20/584
Inventor 尚保昌张良刘建辉乔坤胡秋歌李尚
Owner 上海金不换兰考制药有限公司
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