THIODIGLYCOLIC ANHYDRIDE synthesis
- Product Name:THIODIGLYCOLIC ANHYDRIDE
- CAS Number:3261-87-8
- Molecular formula:C4H4O3S
- Molecular Weight:132.14
Yield:3261-87-8 98%
Reaction Conditions:
at 55 - 65; for 2.75 h;Temperature;
Steps:
1-3; 1-3 A preparation method of thioglycolic acid anhydride includes the following steps:
1) The vaporization of trifluoroacetic anhydride: the trifluoroacetic anhydride is vaporized in a vaporization device and is ready for use;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 into 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 the gas detector. When the gas detector shows that there is no air in the suspended gas-solid reaction device, continue to pass the vaporized trifluoroethane The acid anhydride can make the powder thiol diacetic acid be stably suspended in the high-temperature trifluoroacetic acid gas flow (this value is set in advance before the reaction starts, and is recorded by the gas flow detector and transferred to the controller for storage), from the suspension The feed port on the top of the gas-solid reaction device is intermittently fed with 500g of sulfidiacetic acid. After 45 minutes of sulfidiacetic acid is added, the reaction is carried out at 55°C for 1 hour. Multiple thermocouples are heated to increase the temperature. When the temperature in the reaction device reaches 65°C, the heating is stopped, so that after the reaction is reacted at this temperature for 1 hour, the vaporized trifluoroacetic anhydride is stopped from the gas inlet. Even stop heating, and export the obtained solid product from the discharge port provided at the bottom of the suspended gas-solid reaction device;3) Purification of thioglycolic anhydride: the solid product was washed once with 200 mL of refrigerated anhydrous petroleum ether, and then washed once with 200 mL of refrigerated anhydrous ether to obtain 431.2 g of pure thioglycolic anhydride, with a yield of 98 %.
References:
Wuhan Benjamin Pharmaceutical Co., Ltd.;Hu Kexiong;Wang Yuqin CN111995614, 2020, A Location in patent:Paragraph 0037-0052; 0060-0065
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