Improved propacetamol hydrochloride preparation process

A technology of propetamol hydrochloride and propetamol, which is applied in the field of synthesis of organic compounds with carbocyclic rings, can solve the problems of difficulty in the refining process, high requirements for raw and auxiliary materials, and many times of refining, and achieve operational process Easier to control, reduce product cost, and reduce the effect of many by-products

Inactive Publication Date: 2016-01-06
蚌埠丰原涂山制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method still has disadvantages: 1. It has high requirements on the raw and auxiliary materials used in production; 2. The refining process is difficult to succeed at one time, and often requires 2-3 times of refining to obtain the ideal product; 3. Due to the number of times of refining More, the product yield is relatively low

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  • Improved propacetamol hydrochloride preparation process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1. Add 120kg of acetone and 10kg of acetaminophen to a 200L reactor, stir to dissolve, add 24kg of anhydrous potassium carbonate, stir and cool. Control the temperature of 15-20 DEG C to add 7.5 kg of chloroacetyl chloride dropwise, and complete the dropwise addition in 1.8 hours, and control the temperature for 1.5 hours to complete the reaction. Add 0.5 kg of potassium iodide and control the temperature at 15-20°C and add 11.5 kg of diethylamine dropwise. After the addition of diethylamine in 2 hours, the temperature was controlled to react for 50 minutes and filtered, and the filter cake was washed with acetone. The collected filtrate was concentrated in vacuo to obtain a viscous crude product of Propatamol.

[0029] 2. Add 40 kg of chloroform and 30 kg of purified water to the viscous crude product of propatamol, stir and purify, extract the chloroform layer, and concentrate the chloroform under reduced pressure to obtain the product of propatamol.

[0030] 3. Add 80kg...

Embodiment 2

[0033] 1. Add 120kg of acetone and 10kg of acetaminophen to a 200L reactor, stir to dissolve, add 24kg of anhydrous potassium carbonate, stir and cool. Control the temperature to 20-25°C and add 7.5kg of chloroacetyl chloride dropwise, and the dropwise addition is completed in 1.6 hours, and the temperature is controlled to react for 1.5 hours, and the reaction is completed. Add 0.5 kg of potassium iodide and control the temperature to 20-25°C and add 11.5 kg of diethylamine dropwise. After the addition of diethylamine in 2 hours, the temperature was controlled to react for 50 minutes and filtered, and the filter cake was washed with acetone. The collected filtrate was concentrated in vacuo to obtain a viscous crude product of Propatamol.

[0034] 2. Add 40 kg of chloroform and 30 kg of purified water to the viscous crude product of propatamol, stir and purify, extract the chloroform layer, and concentrate the chloroform under reduced pressure to obtain the product of propatamol...

Embodiment 3

[0038] 1. Add 120kg of acetone and 10kg of acetaminophen to a 200L reactor, stir to dissolve, add 24kg of anhydrous potassium carbonate, stir and cool. Control the temperature at 20-25°C and add 7.5 kg of chloroacetyl chloride dropwise, and finish the dripping in 1.5 hours, and control the temperature to react for 1.5 hours, and the reaction ends. Add 0.5 kg of potassium iodide and control the temperature at 15-20°C and add 11.5 kg of diethylamine dropwise. After the addition of diethylamine in 2 hours, the temperature was controlled to react for 50 minutes and the filter cake was washed with acetone. The collected filtrate was concentrated in vacuo to obtain a viscous crude product of Propatamol.

[0039] 2. Add 40 kg of chloroform and 30 kg of purified water to the viscous crude product of propatamol, stir and purify, extract the chloroform layer, and concentrate the chloroform under reduced pressure to obtain the product of propatamol.

[0040] 3. Add 80kg of absolute ethanol ...

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Abstract

The invention belongs to the field of synthesis of organic matters with carbon rings and provides an improved propacetamol hydrochloride preparation process. The process comprises: 1) carrying out acylation reaction to synthesize 4-acetamido phenol chloracetate; 2) carrying out ammonolysis reaction on the 4-acetamido phenol chloracetate to synthesize propacetamol; 3) purifying a propacetamol coarse product; 4) synthesizing propacetamol hydrochloride; and 5) carrying out purification on the propacetamol hydrochloride. By virtue of purification treatment on the propacetamol coarse product, the standard-exceeding problem of the propacetamol coarse product in projects such as residues on ignition caused by quality problem of initial and auxiliary materials is solved, and meanwhile, the refining efficiency is improved. The yield of the product improved through the process is remarkably improved: the yield of the product before improvement is about 50-60% and the yield of the product after improvement is about 60-70%.

Description

Technical field [0001] The invention belongs to the field of carbon ring organic synthesis, and is specifically an improved preparation process of propatamol hydrochloride. Background technique [0002] Propatamol hydrochloride, the chemical name 4-acetaminophen diethylamino acetate hydrochloride, is an acetaminophen derivative drug developed by Bumei Squibb (USPA) in recent years. It can be supplied to muscles or Intravenous administration, the blood is rapidly hydrolyzed into acetaminophen by the action of plasma enzymes, thereby overcoming the difficulty of administration due to the instability of acetaminophen and the toxic side effects caused by other administration methods , Can replace lysine acetylsalicylic acid (lysine). It is mainly used for symptomatic treatment of pain, especially pain after surgery and cancer pain. Propatamol hydrochloride is used as an acetaminophen preparation for injection, which solves the problem of insolubility of acetaminophen. Since 2000, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/25C07C231/12C07C231/24
Inventor 张祖扬李保琴王劲松杨进辉
Owner 蚌埠丰原涂山制药有限公司
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