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Method for preparing 2, 4, 5-trichloropyrimidine

A technology of trichloropyrimidine and trichlorouracil, applied in the field of pesticides, can solve the problems of high toxicity, harm to the health of synthesis personnel, and complicated synthesis process, and achieves low production cost, great social and economic benefits, and reasonable process conditions. Effect

Pending Publication Date: 2022-01-11
ZHEJIANG XIANFENG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Pyrimidine compounds are important living substances, which widely exist in living organisms and have attracted extensive attention due to their strong biological activity. 2,4,5-Trichloropyrimidine is a new type of reactive dye intermediate raw material and a new antibacterial and anti-inflammatory chemical Synthetic raw materials for medicines. With the increasing sales of new reactive dyes and new antibacterial and anti-inflammatory drugs, the demand for raw materials required for their synthesis is also increasing. At present, most of the synthesis of 2,4,5-trichloropyrimidine uses chlorine, The synthesis process of thionyl chloride, phosphorus oxychloride and phosgene is cumbersome and highly toxic, which brings certain harm to the health of synthesis personnel

Method used

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  • Method for preparing 2, 4, 5-trichloropyrimidine
  • Method for preparing 2, 4, 5-trichloropyrimidine
  • Method for preparing 2, 4, 5-trichloropyrimidine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039]

[0040] step 1:

[0041] Add 240g dilute sulfuric acid (concentration 9%) to a 500ml four-neck bottle, add 20g uracil, and stir for 20-30min while cooling;

[0042] At a temperature of 10-15°C, add 110g of sodium hypochlorite solution and react until the basic reaction of uracil is detected by HPLC (the content is not more than 1%);

[0043] Heated to reflux for 1-2h, then cooled to 20-30°C, filtered, washed with water, and dried to obtain 24.3g of white powder with a yield of 92.8% and a purity of over 99.5% by HPLC.

[0044] Step 2:

[0045] Add 110g tetrahydrofuran, 48g 5-chlorouracil and 0.6g DMF in the reaction flask, stir to dissolve, then add dropwise the chloroform solution of bis(trichloromethyl)carbonate, wherein the chloroform of bis(trichloromethyl)carbonate Solution is that 79g bis(trichloromethyl)carbonate is dissolved in 150g tetrahydrofuran;

[0046] After completion, heat up to 63-65°C, react until HPLC detects that the basic reaction of uracil i...

Embodiment 2

[0050]

[0051] step 1:

[0052] Add 270L of water to a 500L enamel kettle, add 26kg of 98% sulfuric acid dropwise under ice-salt cooling, cool down to 30-35°C after dropping, and add 30kg of uracil;

[0053] Cool to 15-20°C, slowly add 161 kg of sodium hypochlorite solution under stirring conditions, and stir the reaction until the basic reaction of uracil detected by HPLC is complete (the content is not more than 1%);

[0054]Raise the temperature at 95-100°C to react, after reacting for 3-4 hours, cool to 20-25°C, centrifuge, and dry to obtain 37.4kg of white powder with a yield of 95.3% and a purity of 99.1% by HPLC.

[0055] Step 2:

[0056] With 230kg chloroform, 100kg 5-chlorouracil, 1.1 kg DMF is joined in the 500 L reactor, stirring and dissolving, then add the chloroform solution (163kg bis(trichloromethyl)carbonate) of bis(trichloromethyl)carbonate dissolved in 200kg chloroform).

[0057] After the addition is complete, raise the temperature to 60-65°C and rea...

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Abstract

The invention relates to a method for preparing 2, 4, 5-trichloropyrimidine. The method comprises the following steps that: 1) uracil reacts with sodium hypochlorite under an acidic condition to form 5-chlorouracil; and 2) the 5-chlorouracil and bis (trichloromethyl) carbonate react to form 2, 4, 5-trichlorouracil. The preparation method is high in yield and low in cost, has the advantages of being easy to operate, little in pollution, safe, environmentally friendly and the like, and is suitable for large-scale industrial production. The reaction equation is shown in the specification.

Description

technical field [0001] The invention belongs to the technical field of pesticides and relates to a method for preparing 2,4,5-trichloropyrimidine. Background technique [0002] Pyrimidine compounds are important living substances, which widely exist in living organisms and have attracted extensive attention due to their strong biological activity. 2,4,5-Trichloropyrimidine is a new type of reactive dye intermediate raw material and a new antibacterial and anti-inflammatory chemical Synthetic raw materials for medicines. With the increasing sales of new reactive dyes and new antibacterial and anti-inflammatory drugs, the demand for raw materials required for their synthesis is also increasing. At present, most of the synthesis of 2,4,5-trichloropyrimidine uses chlorine, The synthesis process of thionyl chloride, phosphorus oxychloride and phosgene is cumbersome and highly toxic, which brings certain harm to the health of synthesis personnel. [0003] For example, CN102827085...

Claims

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Application Information

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IPC IPC(8): C07D239/30
CPCC07D239/30
Inventor 熊云茂陈小平王国才王焕挺
Owner ZHEJIANG XIANFENG TECH
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