Preparation method of pharmaceutical-grade ultra-high-purity ethyl pyruvate

An ultra-high-purity technology of ethyl pyruvate, applied in the field of pharmaceutical or pharmaceutical intermediate synthesis, which can solve the problems of high discharge of "three wastes", excessive sulfur content in products, and low product yield.

Pending Publication Date: 2022-06-07
苏州仁晟新材料科技有限公司
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0003] The synthetic method of ethyl pyruvate mainly contains three ways at present: one, tartaric acid dehydration decarboxylation prepares pyruvate, then pyruvic acid and ethanol carry out esterification reaction to produce ethyl pyruvate, and the yield of this method is low, and hydrogen sulfate is used in the process Potassium is used as a dehydrating agent, resulting in excessive sulfur content in the product, and the purity cannot reach the pharmaceutical level; 2. Microbial fermentation method, the product yield is low, and the residual microorganisms cannot be used for downstream drug synthesis, especially for infusion drug products 3. Ethyl lactate oxidation method, which uses chloroform as a solvent and trichloroisocyanuric acid as an oxidant. The "three wastes" discharge in the production process is high, and the chlorine content in the product ethyl pyruvate exceeds the standard, which cannot meet the requirements of pharmaceuticals. Aspects of application

Method used

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Examples

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Effect test

preparation example Construction

[0015] A pharmaceutical grade ultra-high purity ethyl pyruvate preparation method, the composite metal oxide catalyst used is based on molybdenum and vanadium, adding antimony, niobium, bismuth, tungsten, cobalt, nickel, gold, silver, palladium, platinum, rhodium, iridium in one or more metal elements, together form a composite metal oxide catalyst.

[0016]The specific preparation method is: molybdenum salt and vanadium salt massage ratio 1: 0.1-1:1 dissolved in water to form a mixed solution A, and then the molar ratio of molybdenum, niobium, bismuth, tungsten, cobalt, nickel, gold, silver, palladium, platinum, rhodium, iridium dissolved in the above mixed solution A to form a mixed solution B, the molybdenum, vanadium and the added metal elements in solution B the molar ratio of 1: 0.1: 0-1: 1: 0.5. Add oxalic acid solution to mixed solution B to adjust the PH value to neutral, forming mixed solution C. After stirring the above mixed solution C for 1-5 hours, drying at 120 °C f...

Embodiment 1

[0019] 100g ammonium molybdate tetrahydrate and 37.1g ammonium metavanadate were dissolved in 500ml deionized water to form solution A; 12.2g cobalt nitrate hexahydrate was added to solution A and continuously stirred to form solution B; oxalic acid solution was added dropwise in solution B to adjust the PH value to neutral, forming solution C and stirring for 2 hours; then solution C was dried at 120 °C for 12 hours, and the dried solids were roasted at 400 °C and roasted in an air atmosphere for 3 hours. The resulting solid is ground and molded to obtain a composite metal oxide catalyst.

[0020] Take 50g of composite metal oxide catalyst and fill it into a fixed-bed reactor at a temperature of 240 °C, a pressure of 0.15 MPa, and a mass air velocity of ethyl lacticate in the gas phase of 0.1h -1 Under conditions, the mixture of air and ethyl fumogenic lactate with a molar ratio of 5:1 was collected after the reaction was carried out by the catalyst bed. The conversion rate and s...

Embodiment 2

[0022]100g ammonium molybdate tetrahydrate and 33.7g ammonium metavanadate were dissolved in 500ml deionized water to form solution A; 22.5g niobium oxalate was added to solution A and stirred continuously to form solution B; oxalic acid solution was added dropwise in solution B to adjust the PH value to neutrality, forming solution C and stirring for 2 hours. Solution C was then dried at 120 °C for 12 hours, and the dried solids were roasted at 400 °C in an air atmosphere for 3 hours; The resulting solid is ground and molded to obtain a composite metal oxide catalyst.

[0023] Take 50g of composite metal oxide catalyst and fill it into a fixed bed reactor at a temperature of 200 °C, a pressure of 0.2 MPa, and a mass airspeed of ethyl lactate of 0.05 h -1 Under conditions, the mixture of air and ethyl fumogenic lactate with a molar ratio of 4:1 is collected after the reaction through the catalyst bed. The conversion rate and selectivity of the reaction were 99.93% and the selectiv...

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Abstract

The invention discloses a preparation method of pharmaceutical-grade ultra-high-purity ethyl pyruvate, which comprises the following steps: by preparing a composite metal oxide catalyst and taking air as an oxidant, carrying out catalytic oxidation on gas-phase ethyl lactate into ethyl pyruvate through the composite metal oxide catalyst under the conditions that the temperature is 180-300 DEG C and the pressure is 0.1-0.5 MPa, and the conversion rate of the whole process is gt; the selectivity is 99.9%, and the selectivity is 70-90%. The purity gt of the final product ethyl pyruvate after rectification and purification; the purity of ethyl pyruvate is 99.8%, the content of heavy metal, total sulfur and total chlorine is smaller than 1 ppm, the defects of an existing synthesis method are overcome, the purity of ethyl pyruvate reaches the medicine level, and a foundation is laid for application of ethyl pyruvate in medicine synthesis.

Description

Technical field [0001] The present invention relates to the field of pharmaceutical or pharmaceutical intermediate synthesis, in particular to a pharmaceutical grade ultra-high purity ethyl pyruvate preparation method. Background [0002] Ethyl pyruvate is an important pharmaceutical intermediate, which is widely used in drug synthesis: it can be used to synthesize anticonvulsants, anxiety functional tranquilizers, and is used to treat depression; It is also widely used in biological diagnostic reagents and detection reagents, such as for the synthesis of L-tyrosine, L-tryptophan, L-Dopa and biochemical reagents. Its downstream product calcium pyruvate is used in diet pills, which helps to improve the degradation of fat and does not increase the burden on the liver and kidneys, and does not affect the body's storage of proteins; Sodium pyruvate in the infusion component can correct severe metabolic acidosis (such as lactic acidosis and diabetic ketoacidosis) that are not yet clin...

Claims

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Application Information

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IPC IPC(8): C07C67/313C07C69/716C07C67/54
CPCC07C67/313C07C67/54C07C69/716Y02P20/584
Inventor 于彦哲窦和瑞
Owner 苏州仁晟新材料科技有限公司
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