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Synthesis method for D-calcium pantothenate

A synthesis method and technology of calcium pantothenate, applied in the directions of organic chemistry methods, chemical instruments and methods, carboxylic acid amide preparation, etc., can solve the problems of high energy consumption, large pollution, high solvent consumption, etc., and achieve high reaction efficiency and product yield. High, fully converted effect

Active Publication Date: 2018-08-24
安徽省恒锐新技术开发有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In fact, this process has the following disadvantages: one is that the crystallization process of the product requires a low temperature environment, and the energy consumption is high; the other is that the synthesis time is as long as more than 20 hours, which takes a long time, consumes solvents, and causes great pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Embodiment 1: the synthesis of D-calcium pantothenate

[0012] (1) Add 650mL of anhydrous methanol to the reaction vessel, add 580g of D-pantolactone while stirring, then add 2g of activated carbon, stir for 0.5 hours, first coarsely filter, then finely filter, and retain the filtrate to obtain D-pantolide Hydrolyzed acid lactone methanol solution;

[0013] (2) Add 1800ml of anhydrous methanol to the reaction vessel, add 400g of beta-alanine while stirring, and then add 150g of calcium oxide, keep the reaction at 45°C for 2 hours, then add 5g of activated carbon, and stir for 0.5 hours. Filter, then precision filter, retain the filtrate, obtain β-alanine calcium methanol solution;

[0014] (3) the D-pantolactone methanol solution with a volume flow rate of 10ml / min and the β-alanine calcium methanol solution with a volume flow rate of 20ml / min are squeezed into the microchannel flow reactor (Corning Micro Channel reactor, G1 type), the reaction stays at 75-80°C for 15...

Embodiment 2

[0017] Embodiment 2: the synthesis of D-calcium pantothenate

[0018] According to the synthesis method of Example 1, the difference is that the reaction temperature in step (3) is 50-60°C.

[0019] Obtain 1062g white powder product by reaction, carry out physical and chemical detection to the product, the result is as follows: D-calcium pantothenate content is 89.0%, melting point 153-206.5 ℃, specific rotation [α]D 23 =+21.5°(C=1,H 2 O), the conversion rate of D-pantothenate lactone is 90%, and the D-calcium pantothenate productive rate is 89%.

Embodiment 3

[0020] Embodiment 3: the synthesis of D-calcium pantothenate

[0021] According to the synthesis method of Example 1, the difference is that the reaction temperature in step (3) is 100-120°C.

[0022] Obtain 1082g off-white powdery product by reaction, carry out physical and chemical detection to product, the result is as follows: D-calcium pantothenate content is 84.0%, fusing point 160-201.5 ℃, specific rotation [α]D 23 = +17.5°(C=1,H 2 O), the conversion rate of D-pantothenolactone is 100%, and the D-calcium pantothenate productive rate is 85%.

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Abstract

The invention relates to the technical field of chemical production, in particular to a synthesis method for D-calcium pantothenate. The synthesis method comprises the following steps: (1) dissolvingD-pantoyl lactone with absolute methanol to obtain a D-pantoyl lactone methanol solution; (2) reacting beta-alanine and calcium oxide in absolute methanol to obtain a beta-calcium alanine methanol solution; and (3) leading the D-pantoyl lactone methanol solution and the beta-calcium alanine methanol solution into a micro channel flow reactor to mix, and reacting a mixed solution at a temperature being 50-120 DEG C for 5-30 minutes to obtain D-calcium pantothenate. The synthesis method provided by the invention has the advantages of being short in time consumption and high in yield.

Description

technical field [0001] The invention relates to the technical field of chemical production, in particular to a method for synthesizing D-calcium pantothenate. Background technique [0002] Calcium D-pantothenate, also known as vitamin B5. As a component of coenzyme A, D-calcium pantothenate participates in the metabolism of carbohydrates, fats and proteins in the body. It is an indispensable trace substance for maintaining normal physiological functions of humans and animals. It is widely used in the fields of medicine, food and beverage additives, etc. The market demand potential is huge. [0003] In the prior art, the main process for producing D-calcium pantothenate by chemical synthesis is to obtain D-pantoate lactone and β-alanine calcium as raw materials through acylation reaction in a reactor, wherein β-propantoate Calcium phosphate is obtained from the chelation reaction between β-alanine and calcium oxide or calcium hydroxide. In fact, this process has the follow...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/02C07C235/12
CPCC07B2200/07C07C231/02C07C235/12
Inventor 马铭泽马云峰
Owner 安徽省恒锐新技术开发有限责任公司
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