Purification method of 2,4-dichloro-6-styryl pyrimidines

A purification method, pyrimidine-based technology, applied in the direction of organic chemistry, can solve the problems of large solvent consumables, poor separation effect, consumption, etc., and achieve the effect of simple operation, high conversion rate, and simplified operation process

Active Publication Date: 2021-08-27
GUANGDONG UNIV OF TECH
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Problems solved by technology

The chemical polarity of 2,4-dichloro-6-styrylpyrimidines is similar to that of the reaction substrate benzaldehydes, and the separation effect of conventional column chromatography separation technology is poor, and a large amount of solvent consumables are required, which is not necessary. Conducive to the expanded production of 2,4-dichloro-6-styrylpyrimidines

Method used

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  • Purification method of 2,4-dichloro-6-styryl pyrimidines
  • Purification method of 2,4-dichloro-6-styryl pyrimidines
  • Purification method of 2,4-dichloro-6-styryl pyrimidines

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1. Preparation method

[0029] 1) Take by weighing 12.0g sodium hydride that adopts 60% mineral oil to disperse, join in the round-bottomed flask, and feed nitrogen to fully discharge the air in the round-bottomed flask;

[0030] 2) Add 300mL tetrahydrofuran to the round bottom flask, stir at 450prm; then, weigh 22.0g 2,4-dichloro-6-methylpyrimidine, dissolve it in 50mL tetrahydrofuran and add it to the round bottom flask;

[0031] 3) Measure 15mL of p-methoxybenzaldehyde into a round-bottomed flask and react for 8 hours; cool the round-bottomed flask in an ice-water bath for 10 minutes, and add a small amount of water dropwise until no bubbles are generated;

[0032] 4) Take the reaction product in the reaction system, add 400mL of dichloromethane and 400mL of water for liquid separation and extraction, repeat the operation three times, and combine the organic phase; dry the organic phase with anhydrous magnesium sulfate, filter to obtain anhydrous organic phase, organ...

Embodiment 2

[0042] In this embodiment, multiple sets of composite solvents are used to replace the dichloromethane-ethanol (1:1, v / v) in Step 2 of Example 1, and the crystallization effect is shown in Table 1:

[0043] Table 1

[0044]

[0045]

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Abstract

The application belongs to the technical field of medicinal chemistry, and specifically relates to a purification method of 2,4-dichloro-6-styryl pyrimidine compounds. The purification method provided by the present invention is: dissolving the crude product containing 2,4-dichloro-6-styryl pyrimidines in dichloromethane, adding ethanol equal to the volume of dichloromethane, mixing, and placing Volatilize in a ventilated place at a preset temperature to precipitate crystals; filter, collect the crystals, and wash the crystals with a small amount of ethanol to obtain high-purity crystalline products 2,4-dichloro-6-styrylpyrimidines. Compared with the prior art, the purification method of 2,4-dichloro-6-styryl pyrimidines provided by the present invention is easy to operate and has a high conversion rate; moreover, it does not need to consume a large amount of solvent, and the product has high purity, which is beneficial to Expanded production of 2,4-dichloro-6-styrylpyrimidines.

Description

technical field [0001] The invention belongs to the technical field of medicinal chemistry, and in particular relates to a purification method of 2,4-dichloro-6-styryl pyrimidine compounds. Background technique [0002] 2,4-dichloro-6-styrylpyrimidine compounds are generally used as chemical intermediates for the synthesis of pharmaceutical intermediates. The two chlorine atoms in its structure have activity differences, and different groups can be selectively substituted at the 2nd and 4th positions to obtain derivatives with huge structural differences, which can be used for androgen receptor inhibitors and golden yellow The intermediate synthesis of staphylococcal dihydrofolate reductase inhibitor has important economic value. [0003] At present, 2,4-dichloro-6-styrylpyrimidines are mainly prepared by reacting benzaldehydes and 6-methyl-2,4-dichloropyrimidine under alkaline conditions, and then through column chromatography Separation technology separates and purifies ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D239/30
CPCC07D239/30
Inventor 江政云赵肃清张焜杨洋张炳杰高鸿灿姚锐明
Owner GUANGDONG UNIV OF TECH
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