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Synthetic method of dimethyl cysteamine hydrochloride

A technology of dimethylcysteamine hydrochloride and its synthesis method, which is applied in the field of synthesis of dimethylcysteamine hydrochloride, can solve problems such as long reaction cycle and unsatisfactory product quality, and achieve low component cost , Low requirements for reaction equipment and simple reaction process

Active Publication Date: 2012-05-02
山东胜利生物工程有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method has mild conditions and low cost. Although it is improved compared with the previous several processes, the reaction cycle is long and the product quality still cannot meet the requirements.

Method used

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  • Synthetic method of dimethyl cysteamine hydrochloride
  • Synthetic method of dimethyl cysteamine hydrochloride
  • Synthetic method of dimethyl cysteamine hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1. Synthesis of 5,5-dimethyl-2-isopropylthiazoline reaction

[0034] In the autoclave, 144g of isobutyraldehyde, 81g of triethylamine, and 32g of elemental sulfur were mixed uniformly.

[0035] Discharge the mixed gas to -0.05MPa by vacuum decompression, open the circulating cooling water, keep the temperature below 40°C, feed ammonia gas to pressurize to 0.03MPa, stop feeding ammonia gas, open the vent valve, and discharge excess ammonia gas to Normal pressure, repeated charging and discharging 5 times, finally reaching normal pressure after deflation.

[0036] Keep circulating cooling water and continue to fill with 34gNH 3 , close the intake valve, stop cooling, start heating to 110°C, and keep for 4h. Stop heating, turn on circulating cooling water, cool down to 20°C, and repeat the above process.

[0037] Stop the reaction, open the inlet valve, release the product under pressure, the solution is light yellow or brown. After filtration, let it stand for liqui...

Embodiment 2

[0046] 1. Synthesis of 5, 5-dimethyl-2-isopropylthiazoline reaction

[0047] In the autoclave, 144g of isobutyraldehyde, 81g of triethylamine, and 32g of elemental sulfur were mixed evenly.

[0048] Use vacuum to depressurize to -0.05MPa to discharge the mixed gas, open the circulating cooling water, keep the temperature below 40°C, feed ammonia gas and pressurize to 0.03MPa, stop feeding ammonia gas, open the vent valve, and discharge excess ammonia gas to Normal pressure, repeated charging and discharging 5 times.

[0049] Keep circulating cooling water, continue to charge 68 g NH 3 ; Close the intake valve, stop cooling, start heating at a rate of 0.5°C / min to 110°C, and keep for 4h.

[0050] Stop the reaction, open the vent valve, and discharge the remaining waste gas of the reaction; open the intake valve, fill with nitrogen and pressurize to discharge the product, the solution is light yellow or brown. After filtering, let stand to separate liquid to remove water ph...

Embodiment 3

[0059] 1. Synthesis of 5, 5-dimethyl-2-isopropylthiazoline reaction

[0060] In the autoclave, 144g of isobutyraldehyde, 81g of triethylamine, and 32g of elemental sulfur were mixed evenly.

[0061] Use vacuum to depressurize to -0.05MPa to discharge the mixed gas, open the circulating cooling water, keep the temperature below 40°C, feed ammonia gas and pressurize to 0.03MPa, stop feeding ammonia gas, open the vent valve, and discharge excess ammonia gas to Normal pressure, repeated charging and discharging 5 times.

[0062] Keep circulating cooling water and continue to fill with 51 g NH 3 ; Close the intake valve, stop cooling, start heating at a rate of 0.5°C / min to 100°C, and keep for 8 hours.

[0063] Stop the reaction, open the vent valve, and discharge the remaining waste gas of the reaction; open the intake valve, fill with nitrogen and pressurize to discharge the product, the solution is light yellow or brown. After filtering, let stand to separate liquid to remo...

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Abstract

The invention discloses a synthetic method of dimethyl cysteamine hydrochloride. The method comprises the following steps of: synthesizing 5,5-dimethyl-2-isopropyl thiazoline by taking isobutylaldehyde, element sulfur, ammonia gas and triethylamine as raw materials; reducing the 5,5-dimethyl-2-isopropyl thiazoline into 5,5-dimethyl-2-isopropyl thiazolidine under the actions of sodium borohydride and acid; and reacting the 5,5-dimethyl-2-isopropyl thiazolidine and phenyl hydrazine under the air insulating situation to obtain dimethyl cysteamine hydrochloride. The method has the advantages of readily-available reaction raw materials, easiness for operating the reaction process, low requirement on the reaction equipment, relatively mild reaction conditions, feeding of the product of every step of reaction into a next step reaction after refining and purifying, high yield and high purity, and the purity of the finally-obtained dimethyl cysteamine hydrochloride is close to 100 percent.

Description

technical field [0001] The invention relates to a method for synthesizing dimethyl cysteamine hydrochloride. Background technique [0002] Cysteamine hydrochloride (CSH) is an important chemical raw material and pharmaceutical intermediate, the molecular formula is C 2 h 7 NSHCl has important physiological functions and good complexation properties, and is widely used in cosmetics, medicine, animal feed additives, and biological materials such as alkylation, biochips, and biochemical pharmaceuticals. Dimethylcysteamine hydrochloride is a kind of CSH. It is an important chemical raw material and pharmaceutical intermediate. [0003] The synthesis methods of CSH are divided into biological synthesis and chemical synthesis. Now the domestic main method is chemical synthesis, ethanolamine-hydrogen bromide method, ethanolamine-sulfuric acid-cyclohexylamine method, hydrogen sulfide-aziridine method, ethanolamine-sulfuric acid=thiosulfate method, but these methods may produce ...

Claims

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Application Information

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IPC IPC(8): C07C319/02C07C323/25
Inventor 马景武王永恒李明王炜翟婷马建国
Owner 山东胜利生物工程有限公司
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