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Trimethyl orthoacetate synthesis method

A technology of trimethyl orthoacetate and synthesis method, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry and other directions, can solve the problems of high processing cost, large steam consumption, no process value, etc., and achieves improved mixing. The effect of reducing the water content of the system and improving the reaction yield

Active Publication Date: 2016-03-09
JIANGSU YANGNONG CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] This method consumes a lot of steam, and the raw ester synthesis is a low-temperature reaction through hydrogen chloride; the treatment cost is high and the effect is not obvious
So this method has no technological value

Method used

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  • Trimethyl orthoacetate synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) Put 82kg of acetonitrile, 67.2kg of anhydrous methanol and 300kg of n-hexane in a 1.5m high 1000L enamel reaction kettle equipped with a stirrer and a temperature measuring probe, stir and cool the reaction solution to -10°C, and stir Add 0.085kg of water-absorbing surfactant cetyltrimethylammonium chloride under the state, slowly feed 85kg of dry hydrogen chloride gas, and fully stir and react for 6 hours to form a salt after passing through to obtain alkyliminoacetate hydrochloride Salt.

[0026] 2) Add 160 kg of anhydrous methanol to the alkylimino acetate hydrochloride obtained in step 1), and feed ammonia gas to adjust the pH value of the reaction solution to 5.5-6.0. Keeping it unchanged for 15 minutes, the reaction mixture was stirred at 40°C for 4 hours to complete the alcoholysis, the temperature was lowered and filtered to remove salt, and the filtrate was rectified to obtain 233 kg of trimethyl orthoacetate with a content of 98.02% and a yield of 95.16%. ...

Embodiment 2

[0028] 1) Put 82kg of acetonitrile, 69kg of anhydrous methanol and 300kg of n-hexane in a 1.5m high 1000L enamel reaction kettle equipped with a stirrer and a temperature measuring probe, stir and cool the reaction solution to -10°C, Add 0.095kg of water-absorbing surfactant didodecyldimethylammonium chloride, slowly feed 83kg of dry hydrogen chloride gas, and fully stir and react for 6 hours to form a salt after passing through to obtain alkyliminoacetate hydrochloride. Salt;

[0029] 2) Add 160 kg of anhydrous methanol to the alkylimino acetate hydrochloride obtained in step 1), and feed ammonia gas to adjust the pH value of the reaction solution to 5.5-6.0. Keeping it unchanged for 15 minutes, the reaction mixture was stirred at 40°C for 4 hours to complete the alcoholysis, the temperature was lowered and filtered to remove salt, and the filtrate was rectified to obtain 229.6 kg of trimethyl orthoacetate with a content of 97.92% and a yield of 93.67%.

Embodiment 3

[0031] 1) Put 82kg of acetonitrile, 68.5kg of anhydrous methanol and 300kg of n-hexane in a 1.5m high 1000L enamel reaction kettle equipped with a stirrer and a temperature measuring probe, stir and cool the reaction solution to -10°C, and stir Add 0.080kg of water-absorbing surfactant hexafluorobutyl methacrylate under the state, slowly feed 82kg of dry hydrogen chloride gas, fully stir and react for 6 hours to form a salt after passing through, and obtain alkyliminoacetate hydrochloride;

[0032] 2) Add 160 kg of anhydrous methanol to the alkylimino acetate hydrochloride obtained in step 1), and feed ammonia gas to adjust the pH value of the reaction solution to 5.5-6.0. Keeping it unchanged for 15 minutes, the reaction mixture was stirred at 40°C for 4 hours to complete the alcoholysis, the temperature was lowered and filtered to remove salt, and the filtrate was rectified to obtain 227.4kg of trimethyl orthoacetate with a content of 97.99% and a yield of 92.84%.

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Abstract

The present invention provides a trimethyl orthoacetate synthesis method, wherein acetonitrile and methanol are adopted as starting raw materials. The method comprises: 1) when acetonitrile, methanol and a non-polar solvent are subjected to mixing cooling in a reaction kettle to achieve a temperature of -20 to -5 DEG C, adding a small amount of a Gemini surfactant to the system, then introducing dried hydrogen chloride gas to make a molar ratio of acetonitrile to methanol to hydrogen chloride to the surfactant be 1:1-2:1.05-1.5:0.001-0.005 and make a mass ratio of acetonitrile to the non-polar solvent be 1:2-5, and carrying out a complete stirring reaction after introducing the hydrogen chloride gas so as to generate an ethylenediamine methyl ether hydrochloride; and 2) adding methanol having the amount 2-4 times the molar amount of the starting acetonitrile is added to the ethylenediamine methyl ether hydrochloride generated in the step 1), adjusting the pH value of the reaction system to 5-6.5, carrying out an alcoholysis reaction at a temperature of 25-40 DEG C, filtering the alcoholysis product, and refining to obtain the trimethyl orthoacetate. With the method of the present invention, the water content of the original ester synthesis system can be completely reduced so as to significantly improve the trimethyl orthoacetate yield.

Description

technical field [0001] The invention relates to a compound synthesis method, in particular to a new synthesis process of trimethyl orthoacetate. Background technique [0002] Trimethyl orthoacetate, also known as trimethoxyethane, is an important orthoester, easily soluble in alcohol, ether and other organic solvents. In organic synthesis, trimethyl orthoacetate is an acylating agent used in the synthesis of new sweetener sucralose; it is an intermediate raw material for the synthesis of pyrethroid pesticides such as cypermethrin and kungfuthrin; It is an intermediate required for drugs such as pyridine; it can also be used in the dye and perfume industries. [0003] Trimethyl orthoacetate synthetic technology and synthetic method, there are not many domestic and foreign literature reports, all use acetonitrile as raw material, obtain trimethyl orthoacetate through alcoholysis of ethyleneimine methyl ether hydrochloride, and the synthesis yield is 80% ~90%, but the yield i...

Claims

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Application Information

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IPC IPC(8): C07C43/32C07C41/50
Inventor 王东朝杨凡孔勇解春满郭玉波
Owner JIANGSU YANGNONG CHEM
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