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The preparation method of thioglycolic anhydride

A technology of thioglycolic anhydride and thiodiacetic acid is applied in the field of preparation of erdosteine ​​intermediates, and can solve the problems of low quality, long reaction time, low reaction yield and the like of synthesizing erdosteine, and achieves the The effect of improving the reaction efficiency, shortening the reaction time, and increasing the contact area

Active Publication Date: 2022-01-04
武汉本杰明医药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In summary, although the synthetic process of the key intermediate thioglycolic anhydride in the synthesis of erdosteine ​​is simple, there are problems of low reaction yield and long reaction time, and finally how to obtain high-quality, high-yield The problem of thioglycolic anhydride leads to the problem of low quality and low yield of subsequent synthesis of erdosteine

Method used

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  • The preparation method of thioglycolic anhydride
  • The preparation method of thioglycolic anhydride
  • The preparation method of thioglycolic anhydride

Examples

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Embodiment 1

[0039] A preparation method of thioglycolic anhydride, comprising the following steps:

[0040] 1) Vaporization of trifluoroacetic anhydride: vaporize trifluoroacetic anhydride in a vaporization device for use;

[0041] 2) Synthesis of thioglycolic anhydride: After preheating the internal temperature of the suspended gas-solid reaction device to 55° C., the vaporized trifluoroacetic anhydride is introduced from the air inlet provided at the bottom of the suspended gas-solid reaction device. In the suspended gas-solid reaction device, the gas in the suspended gas-solid reaction device is detected by a gas detector. When the gas detector shows that there is no air in the suspended gas-solid reaction device, continue to feed the vaporized trifluoroethylene Acid anhydride to the flow rate that can make the powder thiodiacetic acid can be stably suspended in the high-temperature trifluoroacetic acid airflow (this numerical value is set in advance before the start of the reaction, a...

Embodiment 2

[0044] A preparation method of thioglycolic anhydride, comprising the following steps:

[0045] 1) Vaporization of trifluoroacetic anhydride: vaporize trifluoroacetic anhydride in a vaporization device for use;

[0046] 2) Synthesis of thioglycolic anhydride: after preheating the internal temperature of the suspended gas-solid reaction device to 45°C, the vaporized trifluoroacetic anhydride is introduced from the air inlet provided at the bottom of the suspended gas-solid reaction device In the suspended gas-solid reaction device, the gas in the suspended gas-solid reaction device is detected by a gas detector. When the gas detector shows that there is no air in the suspended gas-solid reaction device, continue to feed the vaporized trifluoroethylene Acid anhydride to the flow rate that can make the powder thiodiacetic acid can be stably suspended in the high-temperature trifluoroacetic acid airflow (this numerical value is set in advance before the start of the reaction, and ...

Embodiment 3

[0049] A preparation method of thioglycolic anhydride, comprising the following steps:

[0050] 1) Vaporization of trifluoroacetic anhydride: vaporize trifluoroacetic anhydride in a vaporization device for use;

[0051] 2) Synthesis of thioglycolic anhydride: after preheating the internal temperature of the suspended gas-solid reaction device to 50°C, the vaporized trifluoroacetic anhydride is introduced into the In the suspended gas-solid reaction device, the gas in the suspended gas-solid reaction device is detected by a gas detector. When the gas detector shows that there is no air in the suspended gas-solid reaction device, continue to feed the vaporized trifluoroethylene Acid anhydride to the flow rate that can make the powder thiodiacetic acid can be stably suspended in the high-temperature trifluoroacetic acid airflow (this numerical value is set in advance before the start of the reaction, and is recorded by the gas flow detector and passed to the controller for storag...

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Abstract

The invention discloses a preparation method of thioglycolic anhydride, which comprises the following steps: vaporization of trifluoroacetic anhydride: vaporizing trifluoroacetic anhydride in a vaporization device for use; synthesis of thioglycolic anhydride: After the internal temperature of the suspended gas-solid reaction device is preheated to 45-65°C, the vaporized trifluoroacetic anhydride is passed into the suspended gas-solid reaction device, and sulfide disulfide is intermittently added from the top of the suspended gas-solid reaction device. Acetic acid, after reacting for 2 hours, stop feeding vaporized trifluoroacetic anhydride from the air inlet, stop heating, and the solid product obtained is derived from the discharge port; the purification of thioglycolic anhydride: use the solid product respectively with refrigerated Wash with anhydrous petroleum ether and anhydrous ether to obtain pure thioglycolic anhydride. The thioglycolic anhydride synthesized by the invention has high purity and high yield, and the erdosteine ​​produced by reacting the thioglycolic anhydride as a raw material with homocysteine ​​thiolactone hydrochloride has a high yield.

Description

technical field [0001] The present invention relates to the preparation of erdosteine ​​intermediate, in particular to a preparation method of thioglycolic anhydride. Background technique [0002] Erdosteine, chemical name: (±)-S-[2-[N-3-(2-oxotetrahydrothienyl)acetamido]]thioglycolic acid, is a kind of mucus-dissolving drug, used for acute Obstructive bronchitis, chronic obstructive bronchitis, bronchial asthma and other diseases cause sticky sputum and difficulty expectoration. [0003] At present, there are multiple synthetic methods as the key intermediate of synthetic erdosteine, thioglycolic anhydride, the most common method is the synthetic method of thiodiacetic acid and acid anhydride or acid chloride, such as: Chem.Pharm.Bull.50( 4) What is disclosed in the 558-562 (2002) article is to react by refluxing sulfidediacetic acid and acetic anhydride for 3 hours under the protection of nitrogen, and then vacuum concentrate after the reaction, and the concentrate is rec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D327/06
CPCC07D327/06
Inventor 胡可雄王玉琴
Owner 武汉本杰明医药股份有限公司
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