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Synthesis method of 2-amino-6-methyl-5-oxo-4-normal propyl-5-triazole [1,5-alpha] pyrimidine

A synthesis method, triazole technology, applied in the field of pesticide additive synthesis, can solve the problems of long reaction time, low yield, poor product quality, etc., and achieve the effects of short reaction time, high yield and good product quality

Inactive Publication Date: 2007-05-09
湖南天成生化科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] However, the general reaction time is long, the yield is relatively low, and the product quality is poor, so it is not suitable for industrial production.

Method used

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  • Synthesis method of 2-amino-6-methyl-5-oxo-4-normal propyl-5-triazole [1,5-alpha] pyrimidine
  • Synthesis method of 2-amino-6-methyl-5-oxo-4-normal propyl-5-triazole [1,5-alpha] pyrimidine
  • Synthesis method of 2-amino-6-methyl-5-oxo-4-normal propyl-5-triazole [1,5-alpha] pyrimidine

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Experimental program
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Effect test

Embodiment 1

[0045] 3, the preparation of 3-dimethoxy-2-methyl-propionic acid methyl ester (I)

[0046] In the dried reaction kettle equipped with a drying tube, add 12kg methyl methacrylate (0.12 kilomolecules), stir, cool to about -5°C, add 20.1kg bromine (0.26 kilomolecules) dropwise, and control the reaction temperature at At about 15°C, the dropwise addition time is 6 hours. After the dropwise addition is completed, the temperature is raised to 25°C and the reaction is continued for 2 hours with stirring. Then 27% sodium methoxide solution (16.1kg sodium methoxide+43.5kg anhydrous methanol) was added dropwise to control the reaction temperature at 40°C. After the dropwise addition was completed, the reaction was continued to stir for 5 hours. After the reaction is complete, add 50L of water and 3.6kg of glacial acetic acid, extract three times with 45L of ethyl acetate, combine the three extracts, wash with 10L of saturated NaCl solution, and remove the anhydrous MgSO 4 dry. Ethyl a...

Embodiment 2

[0049] Preparation of 3,5-diimino-1,2,4-triazole (II)

[0050] Add 23.4kg of concentrated HCl to the glass-lined reaction kettle, cool to about 10°C, add 7.02kg (0.112 kilomolecules) of 85% hydrazine hydrate, stir, and drop dicyandiamide solution (9kg dicyandiamide (0.107 kilomolecules)+ 7L water), the reaction temperature was controlled at 40°C, and the dropwise addition time was controlled at about 1 hour. After the dropwise addition was completed, the stirring reaction was continued for 3 hours. After the reaction was completed, adjust the pH to 10 with liquid caustic soda, and distilled to dryness under reduced pressure. Add 20L of methanol, stir and reflux for 0.5 hour, filter while hot, and place the filtrate to cool and crystallize. Filter and dry to obtain 10.4kg of product (II), mp200-203°C, yield 80.9%.

[0051] IR: v=3400, 1627, 1488, 1060cm -1 .

Embodiment 3

[0053] Preparation of 2-amino-6-methyl-5-oxo-s-triazol[1,5-α]pyrimidine (III)

[0054] Above-mentioned product (II) 3.92kg (0.04 kilogram molecule), join in the reaction kettle through drying, add sodium ethylate solution (2.72kg sodium ethylate+28L dehydrated alcohol), stir solvent, then add above-mentioned product (I) 7.12 kg (0.041 kilomolecules), heated to reflux at 80°C, stirred and reacted for 48 hours, after the reaction was completed, distilled to dryness under reduced pressure, added 40L of water to the residue, stirred the solvent, and added concentrated HCl dropwise to adjust the pH to 6.0. A large amount of precipitate was produced and stirred for 1 hour, filtered, washed twice with 120L of water, washed with 60L of acetone, and vacuum-dried to obtain 5.05kg of product (III), mp325°C, yield 80.5%, content 98%.

[0055] IR: v=3476, 3339, 3235, 1677, 1643, 1346cm -1 .

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Abstract

A process for synthesizing 2-amino-6-methyl-5-oxy-4-n-propyl-S- triazazole [1,5-alpha] pyrimidine from perspex includes such steps as bromination-substitution reaction to obtain compound A, reaction of bicyanoamine on hydrazine hydrate in acidic medium to obtain compound B, condensation reaction Between A and B in alkaline condition to obtain compound C, dissolving in organic solvent, and reacting on bromopropane to obtain said target product. Its advantages are high output rate and quality and low cost.

Description

technical field [0001] The present invention relates to the improvement of the synthetic method of pesticide additives, specifically refers to a kind of 2-amino-6-methyl-5-oxo-4-n-propyl-S-triazol[1,5-α]pyrimidine (also Improved synthetic method of 2-amino-6-methyl-4-n-propyl-(1,2,4)triazole-pyrimidinone (5). Background technique [0002] 2-Amino-6-methyl-5-oxo-4-n-propyl-S-triazol[1,5-α]pyrimidine is a pesticide additive with anti-strain and emetic effects. After the pesticide is added, it can reduce and avoid the poisoning of humans and animals after contact with the pesticide. [0003] The existing synthetic routes are: [0004] Compound (I)+Compound (II)→Compound (III)→Compound (IV) [0005] [0006] 1.3, the preparation of 3-dimethoxy-2-methyl-propionic acid methyl ester (I) [0007] Add bromine and sodium methoxide solution dropwise to methyl methacrylate, the reaction temperature is -10-80°C, and the reaction time is 1-24 hours. [0008] 2.3, Preparation of 5-...

Claims

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Application Information

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IPC IPC(8): C07D487/04C07D239/00C07D249/00
Inventor 苏建勇叶超郑南华叶茜
Owner 湖南天成生化科技有限公司