A kind of production method of folic acid

A production method, folic acid technology, applied in the direction of organic chemistry, etc., can solve the problems of complex process and high production cost

Active Publication Date: 2019-07-19
JIHENG PHARMA HENGSHUI CITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the two methods not only have high production costs and complicated processes, but also cannot fundamentally reduce the generation of wastewater.

Method used

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  • A kind of production method of folic acid
  • A kind of production method of folic acid
  • A kind of production method of folic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] In this embodiment, in the crude product synthesis step, the relationship of the total amount of materials is as follows:

[0037] N-(p-aminobenzoyl)-L-glutamic acid: 26.6kg;

[0038] 2,4,5-triamino-6-hydroxypyrimidine sulfate: 23.9kg;

[0039] Trichloroacetone crystallization (purity 92%): 25.6kg;

[0040] Sodium metabisulfite: 9.5kg;

[0041] 700L of water;

[0042] Wherein, the material molar ratio relationship is as follows: N-(p-aminobenzoyl)-L-glutamic acid: 2,4,5-triamino-6-hydroxypyrimidine sulfate: trichloroacetone crystallization: sodium pyrosulfite=1: 1:1.6:0.5;

[0043] The volume ratio of the total molar weight of N-(p-aminobenzoyl)-L-glutamic acid to water is 0.14mol / L;

[0044] Materials N-(p-aminobenzoyl)-L-glutamic acid, 2,4,5-triamino-6-hydroxypyrimidine sulfate, trichloroacetone crystals and sodium metabisulfite were added in two batches, the first batch Add 1 / 2 of the total amount of corresponding materials for the first time, and add the remai...

Embodiment 2

[0056] In this embodiment, in the crude product synthesis step, the material relationship is as follows:

[0057] The molar ratio of materials is as follows: N-(p-aminobenzoyl)-L-glutamic acid: 2,4,5-triamino-6-hydroxypyrimidine sulfate: trichloroacetone crystallization: sodium pyrosulfite=1:1.3: 2:0.5;

[0058] The volume ratio of the total molar weight of N-(p-aminobenzoyl)-L-glutamic acid to water is 0.1mol / L;

[0059] Among them, the materials N-(p-aminobenzoyl)-L-glutamic acid, 2,4,5-triamino-6-hydroxypyrimidine sulfate and sodium pyrosulfite are added in two batches. Add 2 / 3 of the total amount of corresponding materials for the first time, and add the remaining materials in the second batch.

[0060] After the first batch of material is added, adjust the pH value between 3.0-3.5 with 10wt% sodium carbonate solution, and control the reaction system pH between 3.0-3.5 in the reaction process, LC-MS detects the above-mentioned system, when N- Add the second batch of mat...

Embodiment 3

[0065] In this embodiment, in the crude product synthesis step, the material relationship is as follows:

[0066] The molar ratio of the materials is as follows: N-(p-aminobenzoyl)-L-glutamic acid: 2,4,5-triamino-6-hydroxypyrimidine sulfate: trichloroacetone crystallization: sodium metabisulfite=1:2: 3:0.8;

[0067] The volume ratio of the total molar weight of N-(p-aminobenzoyl)-L-glutamic acid to water is 0.08mol / L;

[0068] Among them, the materials N-(p-aminobenzoyl)-L-glutamic acid, 2,4,5-triamino-6-hydroxypyrimidine sulfate and sodium metabisulfite are added in three batches. Add 1 / 2 of the total amount of corresponding materials for the first time, add 1 / 2 of the remaining materials for the second batch, and add the remaining materials for the third batch.

[0069] The first batch of reaction temperature is 35°C, after the first batch of materials are added, adjust the pH value to between 3.0-3.5 with 10wt% sodium carbonate solution, and control the pH of the reaction...

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Abstract

The invention relates to a production method folic acid. The production method sequentially includes following steps: synthesizing a crude product: using N-(p-aminobenzoyl)-L-glutamic acid shown as a compound A in a formula I, 2, 4, 5-triamino-6-hydroxy pyrimidine sulfate shown as a compound B in the formula I and trichloroacetone shown as a compound C in the formula I as raw material, sodium metabisulfite as an antioxidant and water as a solvent, and adopting a mode of charging in batches for graded cyclization reaction to obtain reaction liquid; subjecting the reaction liquid to cooling and press filtering to obtain a crude folic acid product; subjecting the crude folic acid product to acid dissolution, alkali dissolution and refining to obtain the folic acid. The mode of charging in batches is adopted to maintain concentration of materials in the reaction liquid within a reasonable range, so that water amount needed at the stage of synthesizing the crude folic acid product is reduced to 1 / 4 of that needed by existing synthesis processes.

Description

technical field [0001] The invention belongs to the field of production of medical raw materials, and mainly relates to a production method of folic acid. Background technique [0002] Folic acid (C 19 h 19 N 7 o 6 ), also known as vitamin B9, is a water-soluble vitamin, which is an anti-anemia drug and is used in the fields of feed, medicine and food. Folic acid is generally a light orange-yellow crystal or flake, carbonized and darkened at about 250°C, and easily soluble in ethanol, carbonated alkali solution, etc. [0003] It is named folic acid because of its rich content in the green leaves of plants. Among the animal tissues, the liver contains the most abundant folic acid. At first, it was extracted from the liver, but now it is mostly produced by synthetic methods. The more commonly used folic acid production technology includes three stages: crude product synthesis, acid-soluble refining and alkali-soluble refining. Wherein, crude product synthesis is to ado...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D475/04
CPCC07D475/04
Inventor 吕学松刘晓莲张晓阳刘毅陈红刘培臻
Owner JIHENG PHARMA HENGSHUI CITY
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