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Preparation method of 2,4,5-triamino-6-hydroxypyrimidine sulfate and folic acid

A technology of hydroxypyrimidine and triamino, which is applied in the preparation of folic acid, 2 fields, can solve the problems of serious environmental pollution, many by-products, and large amount of waste water, and achieve the effects of reducing water pollution, increasing production, and reducing emissions

Active Publication Date: 2019-03-29
ZHEJIANG BENLI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has been applied industrially, but there are many by-products and a large amount of waste water. On average, about 200 tons of waste water are produced for every ton of product produced, which seriously pollutes the environment.

Method used

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  • Preparation method of 2,4,5-triamino-6-hydroxypyrimidine sulfate and folic acid
  • Preparation method of 2,4,5-triamino-6-hydroxypyrimidine sulfate and folic acid
  • Preparation method of 2,4,5-triamino-6-hydroxypyrimidine sulfate and folic acid

Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment 1

[0035] Preparation of ZSM-5 molecular sieve: 0.2g NaAlO 2 Dissolve in 45mL deionized water, then add 26mL TPAOH solution; after stirring at room temperature for 15 minutes, add 16g of tetraethyl silicate; after stirring at room temperature for 3 hours, transfer the solution to the reaction kettle, and age at 100°C for 2.5 hours, Get a guide. Then, a mixed solution containing 5.0g PDADMAC (polydimethyldiallylammonium chloride solution), 17.5mL TPAOH (tetrapropylammonium hydroxide) solution and 1.50mL deionized water was slowly added dropwise under stirring into the solution, and the dropwise addition was completed in 1 hour; after stirring at room temperature for 24 hours, the mixture was transferred to the reaction kettle again, and crystallized at 180° C. for 5.5 days. After the crystallization is completed, the Meso-NaZSM-5 molecular sieve is filtered, washed, dried, and calcined at 600° C. for 5 hours to remove the organic template to obtain a ZSM-5 molecular sieve with a ...

specific Embodiment 2

[0036] Preparation of ZSM-5 molecular sieve: 0.1g NaAlO 2 Dissolve in 45mL deionized water, then add 26mL TPAOH solution; after stirring at room temperature for 15 minutes, add 16g of tetraethyl silicate; after stirring at room temperature for 3 hours, transfer the solution to the reaction kettle, and age at 100°C for 2.5 hours, Get a guide. Then, a mixed solution containing 5.0g PDADMAC, 17.5mL TPAOH solution and 1.50mL deionized water was slowly added dropwise to the solution under stirring, and the dropwise addition was completed in 1 hour; after stirring at room temperature for 24 hours, the mixture was transferred to the reaction In the kettle, crystallize at 180°C for 6 days. After the crystallization is completed, the Meso-ZSM-5 molecular sieve is filtered, washed, dried, and calcined at 600°C for 5 hours to remove the organic template to obtain Meso-ZSM-5 with a silicon-to-aluminum ratio of 65.

specific Embodiment 3

[0037] Preparation of ZSM-5 molecular sieve: 0.065g NaAlO 2 Dissolve in 45mL of deionized water, then add 26mL of TPAOH solution; after stirring at room temperature for 15 minutes, add 16g of tetraethyl silicate; after stirring at room temperature for 3 hours, transfer the solution to the reaction kettle, and after aging at 100°C for 2.5 hours, we get Directing agent. Then, a mixed solution containing 5.0g PDADMAC, 17.5mL TPAOH solution and 1.50mL deionized water was slowly added dropwise to the solution under stirring, and the dropwise addition was completed in 1 hour; after stirring at room temperature for 24 hours, the mixture was transferred to the reaction In the kettle, crystallize at 180°C for 6 days. After the crystallization is completed, the Meso-ZSM-5 molecular sieve is filtered, washed, dried, and calcined at 600°C for 5 hours to remove the organic template to obtain Meso-ZSM-5 with a silicon-to-aluminum ratio of 100.

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Abstract

The invention relates to a preparation method of 2,4,5-triamino-6-hydroxypyrimidine sulfate and folic acid. The preparation method comprises the following steps: enabling cyanoacetate and sodium nitrite to be subjected to reaction under the action of an organic solvent and / or an inorganic solvent and an acidic substance to obtain 2-oximidocyanoacetate; then, enabling the 2-oximidocyanoacetate andguanidine hydrochloride to be subjected to reaction under an alkaline condition to obtain 2,4-diamino-5-isonitroso-6-oxopyrimidine; enabling the 2,4-diamino-5-isonitroso-6-oxopyrimidine and hydrogen gas to be subjected to reaction under an alkaline condition by means of action of Pd / C to obtain 2,4,5-triamino-6-hydroxypyrimidine, and adding sulfuric acid to adjust the pH value to obtain 2,4,5-triamino-6-hydroxypyrimidine sulfate; and then, adding trichloroacetone and N-(4-aminobenzoyl)-L-glutamic acid to be subjected to reaction in a buffer solution under the action of a catalyst molecular sieve so as to obtain the folic acid. Based on the process route, the invention explores the influences of different reaction steps and refining conditions on the preparation route of 2,4,5-triamino-6-hydroxypyrimidine sulfate and the folic acid so as to reduce the wastewater pollution while increasing the yield.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical chemical synthesis, and in particular relates to a preparation method of 2,4,5-triamino-6-hydroxypyrimidine sulfate and a preparation method of folic acid. Background technique [0002] Folic acid N-[4-[(2-amino-4-hydroxy-6-pteridinyl)methylamino]benzoyl]-L-glutamic acid, CAS: 59-30-3, molecular weight: 441.4, structural formula as Mode: [0003] [0004] Folic acid, also known as vitamin M, vitamin Be, pteroyl glutamic acid, is an indispensable vitamin for human beings but cannot be synthesized by itself, and is an indispensable component for the normal growth of organisms. Therefore, it is widely used in feed, medicine and food, and is used in large quantities. At present, all folic acid is industrially produced by chemical synthesis method, which consists of 1,1,3-trichloroacetone and N-(4-aminobenzoyl)-L-glutamic acid, 2,4,5-triamino-6 -Hydroxypyrimidine sulfate reaction and then ...

Claims

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Application Information

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IPC IPC(8): C07D239/22C07D475/04B01J29/46B01J29/48
CPCB01J29/46B01J29/48B01J2229/183B01J2229/186C07D239/22C07D475/04
Inventor 顾海宁王佳佳吴政杰余永志孔富强
Owner ZHEJIANG BENLI TECH CO LTD
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