Preparation method of thioglycolic anhydride

A technology of thioglycolic anhydride and thiodiacetic acid, which is applied in the field of preparation of erdosteine ​​intermediates, can solve the problems of low quality, long reaction time, and low reaction yield in the synthesis of erdosteine, and achieve Improved reaction efficiency, shortened reaction time, and improved contact area

Active Publication Date: 2020-11-27
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

Method used

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  • Preparation method of thioglycolic anhydride
  • Preparation method of thioglycolic anhydride
  • 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. The method comprises the following steps of: vaporization of trifluoroacetic anhydride: vaporizing trifluoroacetic anhydride ina vaporizing device for later use; synthesis of thioglycolic anhydride: preheating the interior of a suspended gas-solid reaction device to 45-65 DEG C, introducing the vaporized trifluoroacetic anhydride into the suspended-state gas-solid reaction device, intermittently adding thionyl diacetic acid from the top of the suspended-state gas-solid reaction device, reacting for 2 hours, stopping introducing the vaporized trifluoroacetic anhydride from a gas inlet, stopping heating, and leading out an obtained solid product from a discharging port; and purification of thioglycolic anhydride: washing the solid product with refrigerated anhydrous petroleum ether and anhydrous ether respectively to obtain pure thioglycolic anhydride. The thioglycolic anhydride synthesized by the method is high inpurity and high in yield; and the yield of erdosteine prepared by reacting the thioglycolic anhydride serving as a raw material with homocysteine thiolactone hydrochloride is high.

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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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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