A method for preparing 3-mercapto-5-methyl-1,2,4-triazole from triazine ring

A triazine ring and triazole technology, applied in the field of organic chemical synthesis, can solve the problems of high process complexity and low conversion rate, and achieve the effects of simple process flow, less environmental pollution, and less waste

Active Publication Date: 2021-08-03
SHANDONG HUIHAI PHARMA & CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the deficiencies in the prior art, the present invention provides a method for preparing 3-mercapto-5-methyl-1,2,4-triazole from a triazine ring. The process is simple and the conversion rate is high. Low conversion rate and high process complexity in the synthetic route

Method used

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  • A method for preparing 3-mercapto-5-methyl-1,2,4-triazole from triazine ring
  • A method for preparing 3-mercapto-5-methyl-1,2,4-triazole from triazine ring

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Embodiment 1

[0027] A method for preparing 3-mercapto-5-methyl-1,2,4-triazole from a triazine ring, comprising the following steps in turn:

[0028] (1) Take 25.2g of triazine ring, add 352.8g of tap water, start stirring to accelerate the dissolution.

[0029] (2) Add 16.5g of 30% hydrochloric acid to adjust the pH of the solution to 2.5.

[0030] (3) Heat up to 72°C and start reflux for 3 hours.

[0031] (4) Suction filtration at 32°C.

[0032] (5) Distillation under reduced pressure The vacuum degree is -0.065 MPa, the temperature is controlled at 53°C, distill until a white solid appears, and the distillation time is 2.1h.

[0033] (6) Cool down to 18°C ​​and filter with suction to obtain a wet product.

[0034] (7) The product quality after drying was 15.2g, and the product obtained by liquid chromatography was 3-mercapto-5-methyl-1,2,4-triazole, the product purity was 99.5115%, and the conversion rate was 83 %.

Embodiment 2

[0036] A method for preparing 3-mercapto-5-methyl-1,2,4-triazole from a triazine ring, comprising the following steps in turn:

[0037] (1) Take 19.3g of triazine ring, add 270.2g of tap water, start stirring to accelerate the dissolution.

[0038] (2) Add 11.1g of 30% hydrochloric acid to adjust the pH of the solution to 2.5.

[0039] (3) Heat up to 72°C and start reflux for 3 hours.

[0040] (4) Suction filtration at 30°C.

[0041] (5) Distillation under reduced pressure The vacuum degree is -0.068 MPa, the temperature is controlled at 51°C, distill until a white solid appears, and the distillation time is 2h.

[0042] (6) Cool down to 16°C and filter with suction to obtain a wet product.

[0043] (7) The product quality after drying was 11.87g, and the product obtained by liquid chromatography was 3-mercapto-5-methyl-1,2,4-triazole, the product purity was 99.5431%, and the conversion rate was 85 %.

[0044] pass figure 1 and figure 2 Two liquid phase detection spect...

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Abstract

The invention discloses a method for preparing 3-mercapto-5-methyl-1,2,4-triazole from a triazine ring, comprising the following steps in sequence: (1) dissolving the triazine ring in water to obtain the triazine ring solution; (2) adding acid to the triazine ring solution to adjust the pH value of the solution to 2-3; (3) heating up and refluxing; (4) after refluxing, cooling and solid-liquid separation to obtain a filtrate; (5) decompressing the filtrate Distill until a white solid appears; (6) Cool the temperature for solid-liquid separation to obtain a solid material; (7) Dry to obtain 3-mercapto-5-methyl-1,2,4-triazole. The present invention uses triazine ring as raw material to prepare 3-mercapto-5-methyl-1,2,4-triazole through transformation, the process is simple, the yield is high, the generated three wastes are few, the environmental pollution is small, and the A new efficient and safe preparation method.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, and in particular relates to a method for preparing 3-mercapto-5-methyl-1,2,4-triazole from a triazine ring. Background technique [0002] Triazine ring is an important pharmaceutical and chemical raw material intermediate. Ceftriaxone sodium prepared from triazine ring is the third generation cephalosporin antibiotic. It plays a very important role in national health. [0003] 3-Mercapto-5-methyl-1,2,4-triazole is an intermediate in the synthesis of ribavirin, and is a very important chemical raw material with high economic value and a great demand in the market. The ribavirin synthesized from it, also known as ribavirin and ribavirin, is a broad-spectrum and potent antiviral drug, belonging to synthetic nucleoside drugs, which can inhibit many DNA and RNA viruses. [0004] There are two commonly used methods for synthesizing 3-mercapto-5-methyl-1,2,4-triazole. The first on...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D249/12
CPCC07D249/12
Inventor 张莉华张忠政姜福元张国辉侯绪会黄明路张世凤
Owner SHANDONG HUIHAI PHARMA & CHEM
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