Preparation method of lipoic acid process impurity
A technology for processing impurities and lipoic acid, applied in the direction of organic chemistry, etc., to achieve the effect of single product, high selectivity, and avoiding the formation of impurities
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Embodiment 1
[0020] Put 10.00g (41.5mmol) of ethyl 6,8-dichlorooctanoate, (100mL) water, and 1.83g (45.7mmol) of sodium hydroxide into a 500mL three-necked flask, stir, heat up to 65°C, and react After 3 hours, the reaction was completed, lowered to room temperature, and then slowly added dropwise a solution of 6.64g (207.5mmol) sulfur and 19.92g (83.0mmol) sodium sulfide nonahydrate in water (100mL) that had been prepared in advance. After the dropwise addition was completed, the temperature was raised React at 50°C for 6 hours. After the reaction is complete, cool down to room temperature. Adjust the pH of the system to 1-2 with 10% dilute phosphoric acid prepared in advance. A large amount of off-white solid precipitates. Keep stirring and crystallizing for 0.5 hours and then filter to collect the crude solid. , and then the solid crude product was placed in a 250 mL three-neck flask, recrystallized with an appropriate amount of ethanol and water, and finally 9.08 g of the target impurit...
Embodiment 2
[0026] Put 10.00g (41.5mmol) ethyl 6,8-dichlorooctanoate, (100mL) water, and 1.66g (41.5mmol) sodium hydroxide into a 500mL three-necked flask, stir, heat up to 65°C, and react After 3 hours, the reaction was completed, lowered to room temperature, and then slowly added dropwise a solution of 6.64g (207.5mmol) sulfur and 19.92g (83.0mmol) sodium sulfide nonahydrate in water (100mL) that had been prepared in advance. After the dropwise addition was completed, the temperature was raised React at 50°C for 6 hours. After the reaction is complete, cool down to room temperature. Adjust the pH of the system to 1-2 with 10% dilute phosphoric acid prepared in advance. A large amount of off-white solid precipitates. Keep stirring and crystallizing for 0.5 hours and then filter to collect the crude solid. , and then the solid crude product was placed in a 250 mL three-neck flask, recrystallized with an appropriate amount of ethanol and water, and finally 8.95 g of the target impurity was ...
Embodiment 3
[0028] Put 10.00g (41.5mmol) of ethyl 6,8-dichlorooctanoate, (100mL) water, and 1.74g (43.6mmol) of sodium hydroxide into a 500mL three-necked flask, stir, and raise the temperature to 65°C to react After 3 hours, the reaction was completed, lowered to room temperature, and then slowly added dropwise a solution of 6.64g (207.5mmol) sulfur and 14.95g (62.3mmol) sodium sulfide nonahydrate in water (100mL) that had been prepared in advance. After the dropwise addition was completed, the temperature was raised React at 50°C for 6 hours. After the reaction is complete, cool down to room temperature. Adjust the pH of the system to 1-2 with 10% dilute phosphoric acid prepared in advance. A large amount of off-white solid precipitates. Keep stirring and crystallizing for 0.5 hours and then filter to collect the crude solid. , and then the solid crude product was placed in a 250 mL three-neck flask, recrystallized with an appropriate amount of ethanol and water, and finally 9.26 g of th...
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