A kind of processing method of s-(-)-lipoic acid recycling
A treatment method, lipoic acid technology, applied in chemical instruments and methods, carboxylate preparation, carboxylic acid halide preparation, etc., can solve the problem that S-6,8-dichlorooctanoic acid cannot be reused, S-(-) - Lipoic acid recovery and utilization is difficult, industrial mass production is difficult to repeat, etc., to achieve the effect of low process operation cost, good recycling effect, simple equipment and reagents
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Embodiment 1
[0023] The processing method of a kind of S-(-)-lipoic acid recycling of the present embodiment, its steps are as follows:
[0024] (1) Dissolve 20.6g S-(-)-lipoic acid in 100mL ethyl acetate, then add 6.7g concentration of 30% KOH aqueous solution, stir and react at 45°C for 8h to obtain S-(-)- Lipoic acid reaction solution;
[0025] (2) Pass the above-mentioned S-(-)-lipoic acid reaction solution into an aeration device (aeration can be air, low-concentration oxygen), and aerate for 4 hours; then cool to 0°C, and add dropwise a concentration of 5% Sulfuric acid was added to a pH value of 4 to obtain a yellow paste;
[0026] (3) Dissolve the above yellow paste in toluene, add 7.8g of thionyl chloride dropwise, react at 60°C for 4h; then cool to 10°C, add 12mL of ethanol dropwise and continue to react for 3h to obtain 20.0g of 6, 8-Dichlorooctanoic acid ethyl ester.
[0027] In this example, the yield of ethyl 6,8-dichlorooctanoate was 83%.
Embodiment 2
[0029] The processing method of a kind of S-(-)-lipoic acid recycling of the present embodiment, its steps are as follows:
[0030] (1) Dissolve 20.6g S-(-)-lipoic acid in 100mL toluene, then add 8g concentration of 20% NaOH aqueous solution, stir and react at 50°C for 6h to obtain S-(-)-lipoic acid reaction solution;
[0031] (2) Pass the above-mentioned S-(-)-lipoic acid reaction solution into an aeration device (aeration can be air, low concentration oxygen), and aerate for 2 hours; hydrochloric acid until the pH value of the solution is 2 to obtain a yellow paste;
[0032] (3) Dissolve the above yellow paste in toluene, add 11.7g of thionyl chloride dropwise, react at 60°C for 3h; then cool to 5°C, add 20mL of ethanol dropwise and continue to react for 6h to obtain 21.5g of 6, 8-Dichlorooctanoic acid ethyl ester.
Embodiment 6
[0033] In this example, the yield of ethyl 6,8-dichlorooctanoate was 89%.
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