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D-calcium pantothenate synthesis method

A technology of calcium pantothenate and pantothenic acid, applied in the preparation of carboxylic acid amide optical isomers, organic chemistry, etc., can solve the problems of increased cost, increased production cost, high technical requirements, etc., to solve environmental problems, improve utilization rate, The effect of simple process

Inactive Publication Date: 2006-05-03
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problems in this method are: (1) the isobutyraldehyde-formaldehyde-hydrocyanic acid method will go through multi-step reactions such as methylolation, cyanohydrinization, hydrolysis, lactonization, etc., and highly toxic hydrogen cyanide will be used in the reaction Acid has high technical requirements, which brings great trouble to management and use, and also increases the cost of taking relevant safety measures; (2) isobutyraldehyde-aldehyde acetic acid method has no production value due to the high price of aldehyde acetic acid (3) Although the difficulty of splitting from calcium pantothenate is small, the expense is large, which increases the production cost
(4) Cyanide-containing wastewater is produced during production, and the BOD of the wastewater 5 , CODc r The organic matter load is very high, above 5000mg / L and 8000mg / L respectively, direct discharge will cause environmental pollution, and must be purified

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1) In 135 grams (1.64mol) of 28% methanol solution of sodium methoxide, 74 grams (0.50mol) of diethyl oxalate and 73 grams (1.0mol) of isobutyraldehyde were added with stirring at 10°C, and the reaction was stirred for 2 hours . Then the temperature was raised to 25° C., and 120 grams (0.6 mol) of 20% NaOH solution was added dropwise, and the stirring was continued for 4 to 5 hours after the drop was completed within 15 to 20 minutes. The temperature was raised to 40°C, 134 g (1.65 mol) formaldehyde solution was added dropwise, and the reaction was stirred for 10-12 hours. Then it was cooled to 20°C, 110 mL of concentrated hydrochloric acid was added dropwise, and stirred for another 1.5 hours. Filter to remove NaCl; distill the filtrate to remove methanol, and extract the residue three times with 300ml ethyl acetate. The organic layers were combined and redistilled, and the 100-110°C / 5-10Torr fraction was collected to obtain 62.5 grams of crude product, which was was...

Embodiment 2

[0040] The specific steps are the same as in Example 1, except that 5 grams of guanidine pantoate obtained in step 4) of Example 1 are added to 13ml of 0.5g / ml sodium methylate solution, refluxed for 3 hours, and cooled to below 20°C , then add 60mL of water, with 6M H 2 SO 4 After adjusting the pH to 7.0, add 1 mL concentrated H 2 SO 4 . After completion, it was heated to 65° C. for 1 hour to react. Concentrate under reduced pressure to remove methanol. Then extract twice with 1,2-dichloroethane. The organic layers were combined, and the solvent was removed under reduced pressure to obtain 3.3 g of DL-pantolactone, which was used for further resolution to make full use of the pantolactone.

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Abstract

The invention discloses a synthesis method for D-calcium pantothenate, which comprises: synthesizing keto lactone pantothenate with diethyl oxalate, isobutanal and formaldehyde, reducing said product, using carbamidine carbonate to resolution out D-pantothenic carbonate and L- pantothenic carbonate; preparing the product with D-pantoic lactone, beta-alanine both from D-pantothenic carbonate and calcium metal. This invention avoids the application of hypertoxic sodium cyanide, stabilizes product quality, and increases material utilization ratio.

Description

technical field [0001] The invention relates to a method for synthesizing calcium D-pantothenate. Background technique [0002] Calcium D-pantothenate is a vitamin drug, which is one of the components of coenzyme A in the human body and animals. Its main function is to participate in the metabolism of protein, fat, and carbohydrates, and to treat vitamin B deficiency, peripheral neuritis, and intestinal twist after surgery. Pain, combined with vitamin C can treat diffuse lupus erythematosus. In addition, calcium D-pantothenate can also form high-energy thioester compounds with hydroxy acids, activate weaker acids, and participate in the synthesis of hemoglobin porphyrin frame, which is also indispensable for the normalization of skin and mucous membrane functions, hair coloring and anti-infection What is missing, also has a positive effect in preventing the side effects of streptomycin and kanamycin. In view of the fact that D-calcium pantothenate has two functions of supp...

Claims

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Application Information

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IPC IPC(8): C07C231/20C07C235/12
Inventor 吴天星骆成才商志才
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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