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Preparation method of compound

A technology for compounds and reaction products, applied in the field of preparation of compounds represented by formula 1, can solve the problems of cumbersome process operation, many operation steps, large product loss, etc., and achieve the effect of simplifying process operation, concise synthesis process and improving production efficiency

Active Publication Date: 2015-04-01
湖北华世通生物医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This invention does not find the root cause and solution for the low yield caused by the non-separation of intermediates. The invention only proposes to synthesize the target product in two steps: after the condensation reaction in step 1, the middle of enol sodium salt or enol potassium salt is obtained, and after Filtration, washing, centrifugation, drying, separation and purification of intermediates, and the method of vacuum drying is adopted, and then enters step 2; the final product of step 2 is washed with brine and dried over sodium sulfate to remove water-soluble impurities
However, the two-step method has many steps and the product processing process is complicated, which leads to cumbersome process operations, more solvents used, more energy consumption, increased process costs, and involves unsafe vacuum drying links, which is not environmentally friendly; eventually resulting in large product losses. , affect product yield and quality, and are not conducive to industrial production
[0007] Therefore, the current method for preparing the compound shown in formula 1 still needs to be improved

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0062] a. Synthesis of methyl 2-fluoroacrylate

[0063] Add 184.2g (2.0mol) of methyl fluoroacetate, 256.0g (2.16mol) of dimethyl oxalate and 1104.0g (14.1mol) of dimethyl sulfoxide into a 3000mL reaction flask, replace with nitrogen twice, and stir at room temperature Dissolve, after the reaction solution is dissolved and clarified, start to add 124.3g (2.3mol) of sodium methoxide solid in batches, control the temperature at 15-25 degrees Celsius, and complete the addition after 1 hour, start to concentrate the reaction solution under reduced pressure, vacuum degree ≥ 0.095Mpa, and react The temperature of the liquid is 35 degrees Celsius. After concentrating for two hours, the sampling control is carried out. The content of methanol is 9.4%, and the content of methyl fluoroacetate is 0.3%. 0.1g of p-cresol, then add 60g (2.0mol) of paraformaldehyde in batches, control the temperature at 20-25 degrees Celsius, after the addition is completed, keep stirring for 1 hour, and con...

Embodiment 2

[0067] a. Synthesis of methyl 2-fluoroacrylate

[0068] Add 184.2 g (2.0 mol) of methyl fluoroacetate, 272.0 g (2.3 mol) of dimethyl oxalate and 736.0 g (9.4 mol) of dimethyl sulfoxide into a 3000 mL reaction flask, replace with nitrogen twice, and stir at room temperature Dissolve, after the reaction solution is dissolved and clarified, start to add 161.3g (2.3mol) of potassium methoxide solid in batches, control the temperature at 15-25 degrees Celsius, and complete the addition after 1 hour, start to concentrate the reaction solution under reduced pressure, vacuum degree ≥ 0.095Mpa, and react The temperature of the liquid is 25 degrees Celsius. After concentrating for two hours, the sampling control is carried out. The content of methanol is 8.0%, and the content of methyl fluoroacetate is 0.1%. 0.1 g of butyl-p-cresol, then add 60 g (2.0 mol) of paraformaldehyde in batches, control the temperature at 20-25 degrees Celsius, after the addition is completed, heat and stir for...

Embodiment 3

[0072] a. Synthesis of methyl 2-fluoroacrylate

[0073] Add 184.2g (2.0mol) of methyl fluoroacetate, 256.0g (2.16mol) of dimethyl oxalate and 1104.0g (14.1mol) of dimethyl sulfoxide into a 3000mL reaction flask, replace with nitrogen twice, and stir at room temperature Dissolve, after the reaction solution is dissolved and clarified, start to add 140.5g (2.6mol) of sodium methoxide solid in batches, control the temperature at 5-15 degrees Celsius, and complete the addition after 1 hour, start to concentrate the reaction solution under reduced pressure, vacuum degree ≥ 0.095Mpa, and react The temperature of the liquid is 28 degrees Celsius. After concentrating for two hours, the sampling control is carried out. The content of methanol is 9.0%, and the content of methyl fluoroacetate is 0.05%. 0.1 g of p-cresol, then add 60 g (2.0 mol) of paraformaldehyde in batches, and control the temperature at 10-15 degrees Celsius. -The content of methyl fluoroacrylate is 10.5%, and the yi...

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Abstract

The invention provides a preparation method of a compound as described in the formula 1. The method comprises the steps of (1) contacting a compound as described in the formula 2 and a compound as described in the formula 3 in the existence of alkali to obtain a compound as described in the formula 4; and (2) directly contacting a reaction product obtained in the step (1) and paraformaldehyde to obtain the compound as described in the formula 1, wherein weak acid is added in the reaction product before the reaction product obtained in the step (1) is in contact with the paraformaldehyde so that the residual alkali in the reaction product can be neutralized. By using the method, the compound as described in the formula 1 can be effectively prepared.

Description

technical field [0001] The present invention relates to the field of chemical synthesis, specifically, the present invention relates to the preparation method of the compound represented by formula 1. Background technique [0002] In recent years, compounds represented by formula 1 have been used more and more in the material and pharmaceutical industries. As an important intermediate, it can not only be used to prepare plastic optical fibers, but also play an important role in the optical fiber communication industry; on the other hand, polymers prepared using such intermediates as raw materials can be combined with some highly active drugs to produce It can be used as a delivery medium to enter the human body, thereby excreting some excess potassium and sodium ions from the body. Because it is a polymer, the particles are small and cannot stay in the human body, so it is very easy to be excreted by the human body. Thereby exert medicinal effect. [0003] [0004] Whe...

Claims

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Application Information

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IPC IPC(8): C07C69/653C07C67/333C07C67/48
CPCC07C67/32C07C67/343C07C69/653
Inventor 王念黄焜杨琼峰宋伟
Owner 湖北华世通生物医药科技有限公司
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