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Method for decomposing triazine ring residues to recover methylhydrazine

A technology of triazine ring and methylhydrazine, which is applied in the field of recovery and utilization of by-products of pharmaceutical intermediates, can solve problems such as difficult to handle, large amount of by-products, and low product yield, and achieve the effect of low cost and easy processing

Active Publication Date: 2020-04-03
SHANDONG HUIHAI PHARMA & CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the main problem of the triazine ring in the industrial production process is the low yield of the product, and the yield of the triazine ring can reach 71%. The yield is not high, and the amount of by-products produced during the synthesis process is large and difficult to handle. Under the tense environmental protection situation, it is imperative to effectively recycle and treat triazine ring residues

Method used

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  • Method for decomposing triazine ring residues to recover methylhydrazine

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Add 30g of triazine ring residue, 300g of water, and 2g of copper chloride to the reaction flask, start stirring, raise the temperature to 130°C and keep it warm for 2 hours, add 7.5g of caustic soda after extracting the distillate, and extract methylhydrazine after distillation of aqueous solution.

Embodiment 2

[0022] Add 30 g of triazine ring residue, 400 g of water, and 6 g of copper chloride to the reaction flask, start stirring, raise the temperature to 110° C. and keep it warm for 4 hours. aqueous solution.

Embodiment 3

[0024] Add 30 g of triazine ring residue, 900 g of water, and 1.5 g of copper sulfate to the reaction flask, start stirring, raise the temperature to 90° C. and keep it warm for 5 hours. aqueous solution.

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Abstract

The invention discloses a method for decomposing triazine ring residues to recover methylhydrazine. The method comprises the following steps: adding the triazine ring residues, water and a copper saltinto a reaction bottle, starting stirring, raising the temperature to 80-130 DEG C, performing a reaction for 2-5 h, distilling with the proceeding of the reaction to extract fractions from the reaction bottle, adding an alkali to the fractions, and performing distillation to obtain a mixture of methylhydrazine and water. The byproduct that is the triazine ring residues is hydrolyzed to recover methylhydrazine and used for synthesizing 2-methylthiosemicarbazide, and a triazine ring is further synthesized, so wastes are recycled, the problem that the triazine ring residues are difficult to treat industrially is solved, and cyclic regeneration from the triazine ring residues to methylhydrazine and then to the triazine ring is realized. A solvent is not used, so that the defects that the organic solvent is flammable, combustible and high in cost are overcome; only the triazine ring residues react with water, the copper salt serves as a catalyst, methylhydrazine is recovered and produced,and the triazine ring residues are hydrolyzed into small molecular salt which is easy to treat, so the method has the advantages of safety, environmental friendliness, low cost and suitableness for industrial production.

Description

technical field [0001] The invention belongs to the field of recovery and utilization of by-products of pharmaceutical intermediates, and in particular relates to a method for decomposing triazine ring residues and recovering methylhydrazine. Background technique [0002] Methylhydrazine is an important raw material for the synthesis of 2-methylthiosemicarbazide, and 2-methylthiosemicarbazide is further reacted with diethyl oxalate to synthesize a triazine ring. The triazine ring is the key intermediate for the synthesis of ceftriaxone sodium, and after synthesizing 7-ACT (7-aminoceftriazine) with 7-ACA (7-aminocephalosporanic acid), ceftriaxone sodium can be synthesized with DAMA . Ceftriaxone sodium, also known as ceftriaxone, is a landmark third-generation cephalosporin antibiotic developed by Roche in Switzerland. It was first launched in Switzerland in 1982 and is the first semi-synthetic broad-spectrum long-acting cephalosporin. , mainly used for infections caused by...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C241/02C07C243/14C07C337/06
CPCC07C241/02C07C337/06C07C243/14
Inventor 张国辉姜福元王乐强侯绪会王亮亮付德修张莉华
Owner SHANDONG HUIHAI PHARMA & CHEM
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