Continuous production method of DL-homocysteine thiolactone hydrochloride

A technology of cystine thiolactone and cystine hydrochloride, which is applied in the field of continuous production technology, can solve the problems of not meeting medical standards, heavy metal pollution of lead electrodes, etc., so as to solve the problem of heavy metal pollution, no heavy metal pollution, and improve product quality. Yield effect

Inactive Publication Date: 2020-04-14
ZHEJIANG UNIV OF TECH
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  • Application Information

AI Technical Summary

Problems solved by technology

The production method of DL-homocysteine ​​thiolactone hydrochloride commonly used in industry is to use lead electrode as the cathode to electrolytically synthesize DL-homocysteine ​​thiolactone hydrochloride, but there are also heavy metals in the lead electrode. Contamination, problems with not meeting medical standards

Method used

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  • Continuous production method of DL-homocysteine thiolactone hydrochloride
  • Continuous production method of DL-homocysteine thiolactone hydrochloride
  • Continuous production method of DL-homocysteine thiolactone hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Reactor see figure 1 , using 7 microchannel reactors connected in parallel and then connected to the plate-and-frame electrolyzer.

[0046] 44.7g DL-methionine and mass fraction 95% sulfuric acid enter the cathode liquid storage tank 5 through the feed port 4 according to the molar ratio of 1:5, and after mixing, pass into the microchannel reactor 2 under the action of the pump 3 (multi-module microreactor, Shandong Jinde New Material Co., Ltd.), the reaction temperature is 80°C, and the flow rate in the reactor is controlled at 8ml / min. The reaction solution containing DL-homocystine obtained after the reaction is passed into the liquid storage tank 6, and then goes to the storage tank through the feed port 9. 3M hydrochloric acid is added to the liquid tank 6 at one time, and the molar ratio of the added hydrochloric acid to DL-methionine is 4. The liquid storage tank 6 is also provided with an exhaust port to discharge the waste gas in the reaction liquid. The feed l...

Embodiment 2

[0049] The steps are the same as in Example 1, except that 11 microchannel reactors are connected in parallel to the plate and frame electrolyzer, the molar mass ratio of DL-methionine to sulfuric acid is 1:3, and the reaction temperature is 70°C. The internal flow rate is controlled at 5ml / min, and the condition of the electrolysis part is constant. After dehydration and condensation, cooling and drying, the product is analyzed by high performance liquid chromatography. The product yield is 66.2%, and the product purity is 99.1%.

Embodiment 3

[0051] The steps are the same as in Example 1, the difference is that: 4 microchannel reactors are connected in parallel to the plate-and-frame electrolyzer, the molar mass ratio of DL-methionine to sulfuric acid is 1:7, and the reaction temperature is 90°C. The internal flow rate is controlled at 12ml / min, and the conditions of the electrolysis part are constant. After dehydration and condensation, cooling and drying, the product is analyzed by high-performance liquid chromatography. The product yield is 54.8%, and the product purity is 99.9%.

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Abstract

The invention discloses a continuous production method of DL-homocysteine thiolactone hydrochloride. The method comprises the following steps: (1) continuously introducing DL-methionine as a raw material and 15-18 mol / L sulfuric acid into a liquid-liquid phase micro-channel reactor, carrying out a reaction to generate DL-homocystine, continuously introducing the DL-homocystine-containing reactionliquid flowing out of the liquid-liquid phase micro-channel reactor and hydrochloric acid into the cathode chamber of a plate-and-frame electrolytic cell, carrying out a reduction reaction on the DL-homocysteine in a hydrochloric acid system at a cathode by using graphite electrodes as the cathode and an anode to generate DL-homocysteine hydrochloride, and continuously flowing the DL-homocysteinehydrochloride-containing catholyte back to a the liquid-liquid phase micro-channel reactor, carrying out a reaction, continuously and circularly reacting until the reaction is complete, and collectingthe catholyte after the reaction is completed; and (2) carrying out impurity removal treatment on the catholyte collected in the step (1), and carrying out dehydration condensation to obtain the DL-homocysteine thiolactone hydrochloride. According to the method, the product yield is increased, the product purity is high, and the domestic medicine standard is met.

Description

[0001] (1) Technical field [0002] The invention relates to a continuous production process for synthesizing DL-homocysteine ​​by using a microchannel reactor and electrolytically synthesizing DL-homocysteine ​​thiolactone hydrochloride. [0003] (2) Background technology [0004] DL-homocysteine ​​thiolactone hydrochloride is one of many amino acid derivatives. It is a white crystalline powder. It is an important pharmaceutical raw material, intermediate and pharmaceutical ingredient. It is used for the preparation of erdosteine ​​and other treatments for bronchial diseases. drug. [0005] Butz first proposed the synthesis method of co-heating DL-methionine and sulfuric acid to obtain DL-homocystine, and it is still used today. The theoretical yield of this method using a traditional reactor is only about 55%. TAKEHARA JUN discloses an industrial production method of DL-homocysteine ​​with a yield of 92%. The method is based on co-heating DL-methionine and sulfuric acid, add...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D333/36
CPCC07C319/24C07D333/36C25B3/25C07C323/58
Inventor 褚有群刘子廒陈赵扬
Owner ZHEJIANG UNIV OF TECH
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