Method for preparing 2-chlorine-4, 6-dimethoxy-1, 3, 5-triazine

A dimethoxyl, disubstituted technology, applied in the field of peptide coupling reagents, can solve the problems of high content of by-products, unsuitable for industrial production, etc., and achieve the effect of accelerating the reaction, increasing the yield, and shortening the reaction time

Inactive Publication Date: 2010-01-13
苏州永拓医药科技有限公司
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Problems solved by technology

[0006] The invention provides a preparation method of 2-chloro-4,6-dimethoxy-1,3,5-triazine, the purpose is to solve the existing 2-chlo

Method used

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  • Method for preparing 2-chlorine-4, 6-dimethoxy-1, 3, 5-triazine
  • Method for preparing 2-chlorine-4, 6-dimethoxy-1, 3, 5-triazine
  • Method for preparing 2-chlorine-4, 6-dimethoxy-1, 3, 5-triazine

Examples

Experimental program
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Example Embodiment

[0024] Example 1: A preparation method of 2-chloro-4,6-dimethoxy-1,3,5-triazine

[0025] Materials used: cyanuric chloride: 240kg; hydroxypropyl-β-cyclodextrin (HP-β-CD): 18Kg; methanol: 600kg; sodium bicarbonate: 327kg; water: 100kg; petroleum ether: 600kg

[0026] Process flow: (1) Synthesis reaction: The 2000L reactor is clean, the exhaust gas absorption device is in place, and the thermometer is displayed normally. Add sodium bicarbonate: 327kg, water: 100kg, catalytic amount of catalyst HP-β-CD 18Kg to the reaction kettle, then dissolve 240kg of cyanuric chloride in 600Kg of methanol, and stir to completely dissolve the cyanuric chloride. (25-30°C) slowly drop the methanol solution of cyanuric chloride into the reaction system, and the reaction temperature is always controlled at 25-30°C during the dropping process. At this time, a lot of bubbles are formed in the reaction system (add slowly, control the reaction temperature to avoid the reaction is too violent, because the r...

Example Embodiment

[0029] Example 2: A preparation method of 2-chloro-4,6-dimethoxy-1,3,5-triazine

[0030] A preparation method of 2-chloro-4,6-dimethoxy-1,3,5-triazine consists of the following steps:

[0031] The first step: mixing sodium bicarbonate, water and a catalytic amount of hydroxypropyl-β-cyclodextrin uniformly to obtain a reaction liquid, wherein the mass ratio of water to sodium bicarbonate is 1:9;

[0032] Step 2: Under the condition of 10~15℃, slowly dropwise add methanol solution with cyanuric chloride dissolved in the reaction solution obtained in the first step to generate monosubstituted triazine. The reaction equation is as follows:

[0033]

[0034] Among them, the mass ratio of cyanuric chloride to methanol is 0.35:1, and the mass ratio of cyanuric chloride to sodium bicarbonate is 0.9:1;

[0035] The third step: Raise the temperature to 65°C to continue the reaction of the monosubstituted triazines generated in the third step to form disubstituted triazines to obtain a mixture con...

Example Embodiment

[0039] Example 3: A preparation method of 2-chloro-4,6-dimethoxy-1,3,5-triazine

[0040] A preparation method of 2-chloro-4,6-dimethoxy-1,3,5-triazine consists of the following steps:

[0041] The first step: mixing sodium bicarbonate, water and a catalytic amount of hydroxypropyl-β-cyclodextrin uniformly to obtain a reaction solution, wherein the mass ratio of water to sodium bicarbonate is 1:4;

[0042] The second step: at 20°C, slowly dropwise add a methanol solution dissolved in cyanuric chloride to the reaction solution obtained in the first step to generate a monosubstituted triazine;

[0043] Among them, the mass ratio of cyanuric chloride to methanol is 0.6:1, and the mass ratio of cyanuric chloride to sodium bicarbonate is 0.7:1;

[0044] The third step: raising the temperature to 40° C., allowing the mono-substituted triazine generated in the third step to continue to react to form a di-substituted triazine to obtain a mixture containing the di-substituted triazine.

[0045] Th...

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Abstract

The invention discloses a method for preparing 2-chlorine-4, 6-dimethoxy-1, 3, 5-triazine, mainly comprising the following steps: firstly, mixing sodium bicarbonate, water and catalytic amounts of catalyst hydroxypropyl methyl-beta-cyclodextrin uniformly to obtain a reactive solution, wherein the mass ratio of the water and the sodium bicarbonate is 1:3-1:10;secondly, at the temperature of 0-30 DEG C, slowly dripping a methyl alcohol solution in which cyanuric chloride is dissolved in the obtained solution in the first step to generate mono-substituted triazine, wherein the mass ratio of the cyanuric chloride and the methyl alcohol is 0.3-0.6:1, the mass ratio of the cyanuric chloride and the sodium bicarbonate is 0.7-0.9:1; and thirdly, rising the temperature to 35-70 DEG C to enable the mono-substituted triazine generatd in the third step to continuously react to generate disubstituted triazine so as to obtain a mixture containing the disubstituted triazine. The raw materials used by the invention has low price, the cost of production materials is reduced. Compared with the prior art, the invention has simple process, higher yield of target products and is more suitable for industrialized production.

Description

technical field [0001] The invention relates to a preparation method of 2-chloro-4,6-dimethoxy-1,3,5-triazine, which is mainly used as a peptide coupling reagent. Background technique [0002] 2-Chloro-4,6-dimethoxy-1,3,5-triazine (hereinafter referred to as disubstituted triazine) was first used as a coupling reagent in the process of synthesizing peptide bonds in 1987, and its coupling efficiency and yield It has a high efficiency and can maintain the original optical activity of the reactants. It is considered to be a stable and highly active peptide (peptide) coupling reagent, and can also be used for the synthesis of amide bonds in complex natural products. Compared with other types of coupling reagents, the price of disubstituted triazines is quite low. [0003] The authorized announcement is CN100379729C, and the Chinese invention patent titled "Nitro Compounds and Their Application in the Preparation of Pemetrexed" discloses the synthesis method of pemetrexed disodi...

Claims

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Application Information

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IPC IPC(8): C07D251/26B01J31/06
Inventor 章立万学明许莉于清萍
Owner 苏州永拓医药科技有限公司
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