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Synthesis method of D-calcium pantothenate

A synthesis method and technology of calcium pantothenate, applied in organic chemistry methods, chemical instruments and methods, preparation of carboxylic acid amides, etc., can solve problems such as unsuitability for industrial production, long fermentation cycle, and environmental impact

Pending Publication Date: 2021-03-09
HUANGGANG MEIFENG CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The current method for preparing D-calcium pantothenate includes adopting the process of obtaining D-pantothenic acid from the fermentation broth, obtaining D-pantothenic acid through resin extraction, and then preparing calcium pantothenate through pantothenic acid. This method has a long fermentation period and low yield. , the operation process is cumbersome, the resin treatment process is complicated, the recycling and waste water discharge is very large, it has a certain impact on the environment, and it is not suitable for industrial production

Method used

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  • Synthesis method of D-calcium pantothenate
  • Synthesis method of D-calcium pantothenate
  • Synthesis method of D-calcium pantothenate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Synthesis of compound Ⅰ (DL-pantothenic acid lactone)

[0052] At room temperature (20-25°C), adjust the pH value of 324kg (37wt%) formaldehyde solution to 9-10 with sodium carbonate (the amount of sodium carbonate is about 36kg), then add 95wt% isobutyraldehyde dropwise into the formaldehyde solution, The temperature is controlled at 20-30°C, and after the dropwise addition is completed, the temperature is raised to 40-50°C for 3 hours;

[0053] Add 600kg of water to the cyanide kettle, and slowly add 200kg of sodium cyanide to make a 30wt% aqueous solution under stirring, then slowly drop the materials in the above condensation kettle into the cyanide kettle under stirring, and control the dropping temperature 10-15°C, dropwise addition time 2-3 hours;

[0054] Add 70wt% sulfuric acid solution to the above cyanidation product, adjust the pH value to be equal to 1-2, heat and control 120 ° C for 2 hours, cool to about 40 ° C, add ammonium bicarbonate to adjust the pH ...

Embodiment 2

[0056] Synthesis of compound Ⅱ (calcium β-alanine)

[0057] At room temperature (20-25°C), add 400L of water and 150kg of ammonium bicarbonate to the reactor, and then slowly drop 80kg of raw acrylic acid into the reactor for 1.5-2 hours. , After the dropwise addition, react for 30 minutes. If there are more bubbles in the reaction, the time should be extended.

[0058] Pump the materials in the batching kettle into the high-pressure reactor, control the temperature of the reactor at 130-140°C, put in 1200L of 25wt% ammonia water, continue to heat the heat transfer oil to 160-170°C, keep the temperature for 3 hours, and then cool down the system to 40-50°C, after the system pressure drops to 0.1MPa, transfer the material to the ammonia recovery kettle, open the ammonia recovery device of the system, control the system temperature to 40-50°C, vacuum degree ≤ -0.085MPa, first Absorb with high-concentration ammonia water for 1 hour, then stir and absorb with low-concentration am...

Embodiment 3

[0062] Synthesis of compound Ⅲ (D-pantolactone)

[0063] Amine salt preparation kettle: Dissolve 215kg of dehydroabietic amine in 400L of methyl tert-butyl ether at room temperature (20-25°C), heat and distill to recover methyl tert-butyl ether until no liquid flows out at 95°C and stop distillation. Then add 600L of water, then use about 27kg of 37wt% hydrochloric acid to adjust the pH value to 3-4, then add 300L of water and transfer to the split kettle for later use.

[0064] Pantothenate hydrolysis kettle: add 500L of water to the kettle, then add 200kg of pantothenic acid lactone, and then use about 65kg of sodium hydroxide to adjust the pH value of the system to 13-14 under stirring, then stir and heat up to 80°C, and keep warm for 30-60 Minutes, then add dilute hydrochloric acid to adjust the pH value of the system to 8-9.

[0065] Put the material in the hydrolysis tank into the split tank and mix it with the prepared amine salt, control the mixing temperature at abou...

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Abstract

The invention discloses a synthetic method of calcium pantothenate, and belongs to the technical field of organic synthesis. The method comprises the following steps: hydrolyzing DLpantothenic acid lactone under an alkaline condition, adding acid after the hydrolysis is finished, then reacting with an organic amine salt in the mixed solvent A, cooling, crystallizing and carrying out solid-liquid separation after the reaction is finished, extracting filter residues by adopting an extracting agent and water under an alkaline condition, separating the extracting agent from an organic phase to obtain organic amine, concentrating a water phase, acidifying, and carrying out reduced pressure distillation to obtain L-pantolactone, carrying out racemization reaction on the L-pantolactone and phosphate to obtain D-pantolactone, extracting the filtrate under an alkaline condition, concentrating the water phase, adding acid, then adding alkali, evaporating the reaction product to dryness, purifying to obtain D-pantolactone, separating the purified mother liquor to obtain DL-pantolactone, wherein the obtained DL-pantolactone is recycled, reacting the beta-calcium aminopropionate with the D-pantolactone in methanol, and crystallizing in the methanol after the reaction is finished to obtain the D-calcium pantothenate.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for synthesizing calcium D-pantothenate. Background technique [0002] Calcium D-pantothenate (D-(+)-N-(2,4-dihydroxy-3,3-dimethylbutyryl)-beta-alanine calcium) is the dextro-isomer calcium salt of pantothenic acid, It is white powder, odorless, with bitter taste, slightly hygroscopicity, most stable when pH value is 5.0-7.0, soluble in glycerin, insoluble in ethanol, chloroform and ether. One of the B vitamins, it is an important raw material for medicine, food, and health care products. [0003] The current method for preparing D-calcium pantothenate includes adopting the process of obtaining D-pantothenic acid from the fermentation broth, obtaining D-pantothenic acid through resin extraction, and then preparing calcium pantothenate through pantothenic acid. This method has a long fermentation period and low yield. , The operation process is cumbersome, the...

Claims

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Application Information

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IPC IPC(8): C07C51/09C07C59/10C07C231/02C07C235/12C07D307/33C07B55/00C07B57/00
CPCC07C51/09C07C231/02C07D307/33C07B55/00C07B57/00C07B2200/07C07B2200/13C07C59/10C07C235/12
Inventor 陈春宏万小攀刘建军
Owner HUANGGANG MEIFENG CHEM TECH
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