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Method for preparing 4,6-dichloropyrimidine

A technology of dichloropyrimidine and dihydroxypyrimidine, which is applied in 4 fields, can solve the problems of low purity and yield, and achieve the effects of reducing costs, reducing processing volume, and reducing dosage

Inactive Publication Date: 2006-09-13
CHONGQING UNISPLENDOUR CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented technology involves preparing certain chemical compounds from specific starting materials through reactions between different substances at high temperatures without generating unwanted side products or losing any desired properties during these processes. By controlling this process conditions, it allows for precise production of various types of molecules that are useful in medicine or other industries such as agriculture, chemistry, biology, etc., while also improving their quality and yields over traditional methods like extraction techniques.

Problems solved by technology

This patents discuss various ways for producing certain types of dyes called fluorescent pigments like quaternary salts containing an organic group attached through carbon atoms between two carboxylic acid groups. These dye molecules exhibit strong absorption at specific frequencies when excited light falls on them. They also emit visible colors under special conditions during excitation.

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0023] Example 1: Add 4,6-dihydroxypyrimidine (27g, 0.24mol, content 98%) in phosphorus oxychloride (108ml, 1.158mol), stir at room temperature for 15min, then add dropwise anhydrous triethyl chloride after drying with caustic potash Amine (67ml, 0.48mol), control the temperature in the reactor at 40-80°C during the dropwise addition, and finish the dropwise addition within about 60 minutes. After the dropwise addition, control the temperature at 60-80°C to continue the reaction for 40 minutes. Cool to 50-60°C, and distill off excess phosphorus oxychloride under reduced pressure. The temperature of vacuum distillation is 60-80°C; Precipitate yellow crystals, control pH = 5-7, directly extract 4,6-dichloropyrimidine with dichloromethane, the extraction temperature is 0-10°C. 33.69 g of light brown solid 4,6-dichloropyrimidine was obtained with a purity of 99.38% and a yield of 95.2%.

Embodiment 2

[0024] Example 2: Add 4,6-dihydroxypyrimidine (27g, 0.24mol, content 98%) in phosphorus oxychloride (108ml, 1.158mol), stir at room temperature for 15min, then add dropwise anhydrous triethyl ether after drying with caustic soda Amine (67ml, 0.48mol), control the temperature in the reactor at 60-90°C during the dropwise addition, and finish the dropwise addition within about 40 minutes. After the dropwise addition, control the temperature at 80-85°C to continue the reaction for 50 minutes. Cool to 55-65°C, and distill off excess phosphorus oxychloride under reduced pressure. The temperature of vacuum distillation is 40-80°C; Control the temperature at 0-5°C, a light yellow solid precipitates, control the pH=5-7, filter, immediately wash twice with ice water, and quickly extract the filtrate twice with 2×50mL chloroform. Then the filter cake was dissolved with 100ml chloroform, the extract and solution were combined, washed once with 10ml saturated sodium chloride solution, dri...

Embodiment 3

[0025] Example 3: Add 84ml of fresh phosphorus oxychloride to 24ml of the recovered phosphorus oxychloride obtained in Example 2 for the treatment of 4,6-dihydroxypyrimidine, the reaction temperature is 40-65°C, and the temperature of vacuum distillation is 50-60°C; The pressure was -0.04~-0.065Mpa, and 22ml of recovered phosphorus oxychloride was obtained. The remaining operations were the same as in Example 2, and 34.46g of light brown solid 4,6-dichloropyrimidine was obtained, with a purity of 99.31% and a yield of 97.21%.

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PUM

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Abstract

A process for preparing 4,6-dichloropyrimidine includes such steps as using phosphoryl chloride to treat 4,6-dihydroxypyrimidine under the existence of anhydrous triethylamine, vacuum distilling for removing excessive phosphoryl chloride, and directly extracting high-purity 4,6-dichloropyrimidine in organic solvent.

Description

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Claims

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Application Information

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Owner CHONGQING UNISPLENDOUR CHEM
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