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Process for preparing 3-amino propane sulfonic acid

A technology of aminopropanesulfonic acid and sulfonation reaction, which is applied in the preparation of sulfonic acid, organic chemistry, etc., can solve the problems such as the inability to obtain a purity greater than 98%, and achieve the effects of mild reaction conditions and simple operation.

Inactive Publication Date: 2003-10-29
四川科伦大药厂有限责任公司
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  • Abstract
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Problems solved by technology

Therefore, if the product prepared by this method is not processed by recrystallization and purification, it is impossible to obtain a product with a purity greater than 98%.

Method used

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  • Process for preparing 3-amino propane sulfonic acid

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Embodiment 1

[0017] Add 15g (0.2mol) of 3-aminopropanol into the reaction flask, add 20ml of concentrated hydrochloric acid and fully stir, then continue to pass in hydrogen chloride to saturation at 40-50°C, and continue to react for 4 hours. Cool to room temperature. And add 75ml of absolute ethanol to dilute, cool to 10°C or lower, a white solid precipitates out. Filter and drain to obtain the intermediate compound of γ-chlorpropanine hydrochloride. After the separation of the intermediate compound, add 10ml of water, and add 30g of Na 2 SO 3 The supersaturated solution of the supersaturated solution was refluxed for 6 hours, and the water was evaporated as much as possible under reduced pressure. After filtering while it was hot, the filtrate was adjusted to pH 6-7 with hydrochloric acid, and 15ml of absolute ethanol was added to dilute it appropriately, so as to obtain a more ideal crystal form , and then cooled to 0°C for crystallization. After filtration, 23 g of 3-aminopropanes...

Embodiment 2

[0020] Add 10 g (0.13 mol) of 3-aminopropanol to the reaction flask while stirring at 50°C and pass in hydrogen chloride until it is no longer absorbed, and react for about 4 hours. 50 ml of 95% ethanol was added to the reactant, cooled to room temperature and then filtered to obtain the intermediate compound of γ-chloralanine hydrochloride. After washing the intermediate compound with 85% ethanol solution, add 5ml of water to dissolve it, and add 20g NaHSO heated to boiling in the intermediate solution under stirring 3 After a concentrated solution, it was refluxed for another 5 hours. After the water was evaporated under reduced pressure, it was filtered while it was hot. After the filtrate was adjusted to neutrality with hydrochloric acid, 10ml of absolute ethanol was added for appropriate dilution, and cooled to 0°C for crystallization. Filtrate to obtain 15g of 3-aminopropanesulfonic acid. During recrystallization, heat to reflux with 200ml of 85% ethanol, cool and crys...

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Abstract

A process for preparing 3-aminopropanesulfonic acid includes introducing hydrogen chloride gas into 3-aminopropanol, diluting with ethanol, cooling to educe out crystal as intermediate, preparing itsaqueous solution, sulfonating reaction with the aqueous solution of alkali-metal sulfite by reflux, acidifying by hydrochloric acid, filtering, and cooling to educe out the crystal of product.

Description

technical field [0001] The invention relates to a method for preparing an intermediate 3-aminopropanesulfonic acid which can be used as a gamma-aminobutyric acid receptor agonist. Background technique [0002] 3-Aminopropanesulfonic acid is a pharmaceutical intermediate used in the preparation of γ-aminobutyric acid receptor agonists. Except for the introduction in Annalen der chemie 565 Bend (22-35), no other preparation reports have been found for the synthesis method of this compound. The synthesis and preparation method reported in this document is to pass ammonia gas into ethanol to make it saturated, add 1,3-propane sultone under cooling, and then raise the temperature to 32°C for reaction to obtain the said product. Since the method uses ethanol as a solvent, the product generated in the reaction is viscous in ethanol, which is easily mixed with unreacted raw materials, the reaction is not easy to complete, and the purification is difficult, and the loss of the produ...

Claims

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Application Information

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IPC IPC(8): C07C303/02C07C309/14
Inventor 张秋材丁敏李文忠程志鹏梁隆
Owner 四川科伦大药厂有限责任公司
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