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Preparation method of 2-chloro-4,6-dimethoxy-1,3,5-triazine

A technology of dimethoxyl and dimethylformamide, applied in the direction of organic chemistry, can solve the problems of troublesome post-processing, high content of monosubstituted triazine, high content of monosubstituted triazine and trisubstituted triazine, and achieve reduction The effect of production cost, improvement of product purity, and simple post-processing

Inactive Publication Date: 2015-09-16
ANHUI SHINDO CHEM
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Problems solved by technology

One is to use cyanuric chloride, sodium carbonate, methanol and water as raw materials to synthesize 2-chloro-4,6-dimethoxy-1,3,5-triazine. This synthetic reaction process needs to be heated to reflux, and the by-product The content of monosubstituted triazine and trisubstituted triazine is high; the other is to use cyanuric chloride and sodium methylate as raw materials and toluene as solvent to synthesize 2-chloro-4,6-dimethoxy-1,3,5 - Triazine, the disadvantage of this method is that the content of monosubstituted triazine and trisubstituted triazine is high, the toluene used as solvent is highly toxic, and the aftertreatment is troublesome, so it is not suitable for industrial production

Method used

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  • Preparation method of 2-chloro-4,6-dimethoxy-1,3,5-triazine

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Embodiment 1

[0018] (1) Preparation of 2-chloro-4,6-dimethoxy-1,3,5-triazine crude product: first add 500kgN,N-dimethylformamide and 369kg cyanuric chloride to the reactor, After the cyanuric chloride is completely dissolved, the reaction kettle is cooled to 5-10°C, and then 245kg of sodium methoxide solid is added. After the addition, it is reacted at room temperature for 2 hours, and then heated to reflux for 2.5 hours. After the reaction, add a large amount of water to the reaction solution , filtered, the obtained solid phase was washed with water, suction filtered, and finally dried to obtain 345kg of crude 2-chloro-4,6-dimethoxy-1,3,5-triazine;

[0019] (2) Purification of crude 2-chloro-4,6-dimethoxy-1,3,5-triazine: Dissolve the obtained crude product in 750kg of heptane for recrystallization, filter, and recover 705kg of heptane from the liquid phase by distillation alkane, and solid-phase drying to obtain 316kg of 2-chloro-4,6-dimethoxy-1,3,5-triazine with a yield of 91.25%.

Embodiment 2

[0021] (1) Preparation of 2-chloro-4,6-dimethoxy-1,3,5-triazine crude product: first add 500kgN,N-dimethylformamide and 369kg cyanuric chloride to the reactor, After the cyanuric chloride is completely dissolved, the temperature of the reaction kettle is lowered to 5-10°C, and then 260kg of sodium methoxide solid is added. After the addition, it is reacted at room temperature for 2 hours, and then the temperature is raised to reflux for 2.5 hours. After the reaction, a large amount of water is added to the reaction solution , filtered, the obtained solid phase was washed with water, suction filtered, and finally dried to obtain 351kg of crude 2-chloro-4,6-dimethoxy-1,3,5-triazine;

[0022] (2) Purification of crude 2-chloro-4,6-dimethoxy-1,3,5-triazine: dissolve the obtained crude product in 750kg heptane for recrystallization, filter, and recover 700kg heptane from the liquid phase by distillation alkane, and solid-phase drying to obtain 313kg of 2-chloro-4,6-dimethoxy-1,3,5-...

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Abstract

The invention discloses a preparation method of 2-chloro-4,6-dimethoxy-1,3,5-triazine, relating to the technical field of organic synthesis. The method comprises the following steps: by using cyanuric chloride and sodium methoxide solid as reaction raw materials and N,N-dimethylformamide as a reaction solvent, gradually heating to obtain a 2-chloro-4,6-dimethoxy-1,3,5-triazine crude product, and finally, recrystallizing with heptane for purification. The reaction temperature is controlled to prepare the product, and the yield is up to 91%. The after-treatment is simple, the heptane recrystallization is utilized to enhance the product purity to 99.5%, and the recovery of the heptane can lower the production cost.

Description

Technical field: [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of 2-chloro-4,6-dimethoxy-1,3,5-triazine. Background technique: [0002] 2-Chloro-4,6-dimethoxy-1,3,5-triazine was first used as a coupling reagent in the process of synthesizing peptide bonds. Its coupling efficiency and yield are high, and it can maintain the original Optical activity, considered a stable and active peptide coupling reagent, can also be used in the synthesis of amide bonds in complex natural products. Compared with other types of coupling reagents, disubstituted triazines are relatively cheap. [0003] At present, there are two main methods for the synthesis of disubstituted triazines. One is to use cyanuric chloride, sodium carbonate, methanol and water as raw materials to synthesize 2-chloro-4,6-dimethoxy-1,3,5-triazine. This synthetic reaction process needs to be heated to reflux, and the by-product The content of monosubst...

Claims

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Application Information

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IPC IPC(8): C07D251/26
CPCC07D251/26
Inventor 刘超郑华忠
Owner ANHUI SHINDO CHEM
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