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Preparation method of high-purity fine sulfanilamide

A high-purity technology of refined sulfonamide, which is applied in the field of preparation of high-purity refined sulfonamide, can solve problems such as waste of by-products, side effects, and reducing the purity of refined sulfonamide intermediates, and achieve the effects of shortening the reaction time, increasing the reaction rate, and reducing the dosage

Active Publication Date: 2013-09-25
中瑞(内蒙古)药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the reasons of reaction temperature, time, stirring and refining in the existing chemical process route, a large number of by-products appear in the process, which not only reduces the purity of DSA intermediates, but also produces a series of waste by-products, which ultimately affects the raw material of hydrochlorothiazide The quality of the drug, causing side effects after taking it to the human body
[0008]CN102675163A (2012-9-19) discloses a preparation method of sulfonamide, but this method is not suitable for the preparation of high-purity sulfonamide

Method used

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  • Preparation method of high-purity fine sulfanilamide
  • Preparation method of high-purity fine sulfanilamide
  • Preparation method of high-purity fine sulfanilamide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Weigh and weigh m-chloroaniline, chlorosulfonic acid, and phosphorus trichloride according to the molar ratio of 1:3:1, and add the m-chloroaniline dropwise to the chlorosulfonic acid at a temperature of 30°C within 1 hour. , and then kept for 5min to obtain the first mixed solution; then the phosphorus trichloride was added dropwise to the first mixed solution at a temperature of 30°C within 1 hour, and stirred for 20min; then the steam was turned on and heated to make the material The liquid temperature rises to 65°C, turn off the steam, and let it heat up naturally until the temperature reaches above 105°C, add cuprous chloride and cuprous bromide, which account for 10% of the mass of m-chloroaniline, and mix according to 1:1, at 105 Keep warm for 3 hours between ℃; then stop stirring, let the feed liquid stand for more than 3 hours, then hydraulically transfer the feed from the chlorosulfonation tank to the high-level storage tank, cool naturally, and water-cool, so ...

Embodiment 2

[0062] Weigh and weigh m-chloroaniline, chlorosulfonic acid, and phosphorus trichloride according to the molar ratio of 1:4:2, and add the m-chloroaniline dropwise to the chlorosulfonic acid at a temperature of 45°C within 2 hours. , and then kept for 20min to obtain the first mixed solution; then the phosphorus trichloride was added dropwise to the first mixed solution at a temperature of 45°C within 2 hours, and stirred for 30min; then the steam was turned on and heated to make the material The liquid temperature rises to 80°C, turn off the steam, and let it heat up naturally, until the temperature reaches above 105°C, add cuprous chloride and cuprous bromide, which account for 30% of the mass of m-chloroaniline, and are mixed according to 1:1, at 110 Keep warm for 3 hours between ℃; then stop stirring, let the feed liquid stand for more than 3 hours, then hydraulically transfer the feed from the chlorosulfonation tank to the high-level storage tank, cool naturally, and water...

Embodiment 3

[0069] Weigh and weigh m-chloroaniline, chlorosulfonic acid, and phosphorus trichloride according to the molar ratio of 1:3.4:1.2, and add the m-chloroaniline dropwise to the chlorosulfonic acid at a temperature of 35°C within 1.5 hours. and keep it for 15 minutes to obtain the first mixed solution; then add the phosphorus trichloride dropwise to the first mixed solution at a temperature of 35° C. within 1.5 hours, and stir for 25 minutes; then turn on the steam and heat to make the material Liquid temperature rises to 70°C, turn off the steam, let it heat up naturally, until the temperature reaches above 105°C, add cuprous chloride and cuprous bromide, which account for 15% of the mass of m-chloroaniline, and mix according to 1:1, at 108 Keep warm for 3 hours between ℃; then stop stirring, let the feed liquid stand for more than 3 hours, then hydraulically transfer the feed from the chlorosulfonation tank to the high-level storage tank, cool naturally, and water-cool, so that ...

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Abstract

The invention relates to a preparation method of fine sulfanilamide and particularly relates to a preparation method of high-purity fine sulfanilamide. The preparation method sequentially comprises the following steps of: proportioning m-chloroaniline, chlorosulfonic acid and phosphorus trichloride, then, mixing chlorosulfonic acid, m-chloroaniline and phosphorus trichloride at the temperature of 30-45 DEG C, heating to 105-120 DEG C and carrying out heat preservation for 2-4hours; standing and cooling to obtain a chlorosulfonated substance; introducing ammonia gas to an amination reaction device for the first time, adding the obtained chlorosulfonated substance, then, introducing ammonia gas to the amination reaction device for the second time, carrying out amination reaction at the temperature of 40-45 DEG C and the pressure of 0.1-0.2MPa, and carrying out heat preservation for 1-3hours to obtain an amide; and carrying out dissolution, decoloration, crystallization and purification on the obtained amide: adding a sodium hydroxide solution to adjust the pH value to 10-11, then, adding active carbon, heating to 80-95 DEG C, carrying out heat preservation for 0.3-0.8h, filter pressing while the solution is hot, adding hydrochloric acid into the obtained filtrate to adjusting the pH to 2-4, separating out white crystal substances, and then, cooling, washing, centrifuging and drying to obtain a finished product of the fine sulfanilamide. The preparation method is few in reaction by-product and high in product purity.

Description

technical field [0001] The invention relates to a preparation method of refined sulfonamide, in particular to a preparation method of high-purity refined sulfonamide. Background technique [0002] Acetyl sulfonamide (chemical name: 4-amino-6-chloro-1,3-benzenedisulfonamide) is an important intermediate in the synthesis of hydrochlorothiazide and chlorothiazide drugs, which are currently the most commonly used diuretics , antihypertensive drugs, have a good effect on the treatment of edema diseases, essential hypertension, central or nephrogenic diabetes insipidus, kidney stones, etc. At the same time, this product is also used in organic synthesis and pesticide intermediates. [0003] The molecular formula is: C 6 h 8 ClN 3 o 4 S 2 ; [0004] Molecular weight: 285.72; [0005] Molecular Structure: [0006] [0007] At present, there are few reports on the synthetic process of fine sulfonamide at home and abroad. The industry generally adopts m-chloroaniline as th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C311/39C07C303/38
Inventor 王建荣徐金保莫胜华王利芳
Owner 中瑞(内蒙古)药业股份有限公司
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