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Preparation method of novel alpha-ketovaline calcium

A technology of ketovaline calcium and temperature control, which is applied in the field of drug synthesis, can solve the problems of high toxicity, many reaction steps, and high cost, and achieve the effects of low toxicity, mild conditions, and easy operation

Active Publication Date: 2014-09-10
SHAOXING MINSHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Route 3 and Route 4 have expensive raw materials, high toxicity, serious pollution, many reaction steps, and high cost, so they are not suitable for industrial production

Method used

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  • Preparation method of novel alpha-ketovaline calcium
  • Preparation method of novel alpha-ketovaline calcium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] at 25 o Under C, drop 300kg of diethyl oxalate into 390kg of sodium methoxide methanol solution, keep stirring for half an hour after dropping, add 180kg of isobutyraldehyde, keep warm for half an hour after adding, at no more than 25 o Under the condition of C, add 500kg of 30% sodium hydroxide aqueous solution, keep it warm for 5 hours after dripping, add 400kg of hydrochloric acid dropwise, stir for half an hour, add 600kg of methyl isobutyl ketone for extraction three times, add 100kg of purified water to the organic phase, and add hydroxide Adjust the pH value to 7.8 with sodium, separate layers, add sodium hydroxide to the organic phase to adjust the pH value to 4.2, separate layers, and combine the aqueous phases. Add sodium hydroxide to the water phase to adjust the pH value to 8.8, and the pH value is not lower than 20 o C was added 300kg calcium chloride aqueous solution, dripped and insulated and stirred for 2 hours, and slowly cooled to 5 o C, keep warm fo...

Embodiment 2

[0032] at 25 o Under C, drop 236 kg of dimethyl oxalate into 486 kg of sodium ethoxide ethanol solution, keep stirring for half an hour after dropping, add 173 kg of isobutyraldehyde, keep warm for half an hour after adding, at no more than 25 o Under the condition of C, add 260kg of 30% sodium hydroxide aqueous solution, keep it warm for 5 hours after dripping, add 400kg of hydrochloric acid dropwise, stir for half an hour, add 600kg of methyl isobutyl ketone for extraction three times, add 100kg of purified water to the organic phase, and add hydroxide Potassium adjusts the pH value of the aqueous solution to 4.5, layering, adding potassium hydroxide to the organic phase to adjust the pH value to 6.5, layering, merging the aqueous phase, adding potassium hydroxide to adjust the pH value to 8.8, and then adding potassium hydroxide to adjust the pH value to 8.8. o C adds 290kg calcium chloride aqueous solution, drips and insulates and stirs for 2 hours, slowly cools down to 5 ...

Embodiment 3

[0035] The only difference between this example and Example 1 is that ammonia water is used instead of sodium hydroxide to adjust the pH value to obtain 193kg of refined dry product with a total yield of 69.6%.

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Abstract

The invention discloses a preparation method of novel alpha-ketovaline calcium, which comprises the steps of: dropping diethyl oxalate into alcoholic solution of metal alkoxide, then dropping isobutyraldehyde, preserving heat and agitating, adding alkali solution, regulating pH after heat preservation, extracting, adding a certain amount of water into the extract, adding alkali liquor for regulating the pH, dropping calcium chloride water solution for salification to obtain crude alpha-ketovaline calcium and then refining the crude alpha-ketovaline calcium in mixed solvent of purified water and organic solvent to obtain refined alpha-ketovaline calcium. The preparation method has the advantages that the reaction conditions are moderate, the operation is simple to conduct, the steps are fewer, the yield is high, the quality is high, the price of the used raw materials is low, no pollution is caused, waste gas and a great quantity of waste residues are not produced and the method is suitable for industrial mass production.

Description

technical field [0001] The invention relates to the technical field of drug synthesis, in particular to a chemical synthesis preparation method of α-ketovaline calcium. Background technique [0002] α-Ketovaline Calcium, English name: α-Ketovaline Calcium, chemical name: 3-methyl-2-oxo-butyrate calcium, CAS: 51828-94-5. α-Ketovaline Calcium is one of the main components of Compound α-Ketoacid Tablets (Kaitong). α-ketoacids and their derivatives have shown increasingly broad application prospects in food, daily chemicals and medicine. In food applications, it can be used as a component of sports nutrition drinks; in functional skin care cosmetics, it can play a very good role in moisturizing, anti-wrinkle, anti-shrinkage, anti-aging and anti-allergy. In medical applications, compound α-ketoacid tablets can treat damage caused by chronic renal insufficiency, and can be used as a specific drug for treating uremia. For patients with renal failure, taking compound α-ketoacid t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C59/185C07C51/41
Inventor 邢亚军傅小明黄希
Owner SHAOXING MINSHENG PHARMA