Method for preparing levodopa by recycling mother liquor
A technology for recycling levodopa and mother liquor, applied in the direction of fermentation, etc., can solve problems such as unfavorable green industrial production, and achieve the effect of reducing processing costs
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Embodiment 1
[0049] 65 g of ammonium chloride, 2 g of ammonium sulfite, 0.125 g of pyridoxal phosphate, 650 g of water, and 50 g of tyrosine phenol lyase were put into a 2-liter four-necked bottle A, and the pH value was controlled to 8.0-8.5 with ammonia water.
[0050] Add 58g of catechol, 55.6g of pyruvate, and 300g of water into a 500mL four-neck bottle B, control the temperature at 20°C, and adjust the pH to 6.8-7.0 with 20% ammonia water to obtain a mixed solution of catechol and ammonium pyruvate.
[0051] Slowly add the liquid in the four-necked bottle B to the four-necked bottle A for about 10 hours. During the dropping process, maintain the temperature at 10-20°C. Add 25g of diatomaceous earth, stir for 30 minutes, filter, and the filtrate is set aside. Add 4g of hydrochloric acid and 200g of drinking water to the filter cake, stir at 50°C for 0.5 hour, filter with suction, and combine the two filtrates. Add dropwise 10% ammonia water to adjust the pH to 6.0-7.0, stir and crysta...
Embodiment 2
[0054] Add the mother liquor C recovered in Example 1 into a 2L reaction flask, add 0.125 g of pyridoxal phosphate, add 1.29 g of ammonium sulfite, add 50 g of tyrosine phenol lyase, and use ammonia water to control the pH value to 8.0-8.5.
[0055] In the 500mL four-necked bottle B, add 58g catechol, 55.6g pyruvic acid, 300g of water steamed from the mother liquor of embodiment 1, control the temperature at 20°C, and adjust the pH to 6.8-7.0 with 20% ammonia water to obtain catechol and A mixed solution of ammonium pyruvate.
[0056] Slowly add the liquid in the four-necked bottle B to the four-necked bottle A. The dropping time is about 10 hours, and the temperature is maintained at 10-20°C during the dropping process. , and add 25g of diatomaceous earth, stir for 30 minutes, filter, and the filtrate is set aside. Add 4g of hydrochloric acid to the filter cake, 200g of water distilled from the mother liquor of Example 1 (that is, for post-treatment beating), stir at 50°C fo...
Embodiment 3
[0059] After the mother liquor is applied mechanically for 20 times (the number of times of the mother liquor is not limited to 20 times), the weight of the mother liquor is 1195g, and the analysis detects that the content of ammonium sulfate is 1.076%, and the content of ammonium sulfate is about 12.86g. Add barium chloride 21.5g to form ammonium chloride and sulfate The barium precipitate is filtered to remove the barium sulfate, and after a large amount of water is evaporated, the temperature is lowered and crystallized to recover ammonium chloride as the amine source for the next batch of reactions.
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