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A kind of environment-friendly preparation method of n,n-dimethylformamide dimethyl acetal

A technology of dimethylformamide and dimethylacetal, which is applied in the preparation of organic compounds, preparation of aminohydroxy compounds, chemical instruments and methods, etc., can solve problems such as unfriendly environment, increase economic benefits and reduce production Effect

Active Publication Date: 2021-10-19
常州沃腾化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The above preparation method uses highly toxic dimethyl sulfate as raw material and produces a large amount of sodium methyl sulfate waste solid, which is not friendly to the environment

Method used

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  • A kind of environment-friendly preparation method of n,n-dimethylformamide dimethyl acetal
  • A kind of environment-friendly preparation method of n,n-dimethylformamide dimethyl acetal
  • A kind of environment-friendly preparation method of n,n-dimethylformamide dimethyl acetal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Drop into 119 grams (1mol) chloroform and 113.4 grams (2.1mol) sodium methylate in the 1L reactor, methyl alcohol 25 grams, kerosene 213 grams, catalyst cuprous chloride 0.6 grams, tetrabutyl ammonium chloride 0.2 grams, close reactor, Turn on the heating, first raise the temperature to about 80°C and react for 2 hours, then slowly raise the temperature to about 120°C and react for 2.5 hours, cool down to below 30°C, press filter, then put the filtrate into the reactor, and feed 90 grams (2mol) of dimethylamine , close the reactor, turn on and heat to 140-150°C for 2 hours, heat preservation reaction for 2 hours, cool down to below 30°C, take a sample for gas phase detection, and deduct the solvent peak: the product purity is 90.5%, chloroform is 5.5%, and trimethyl orthoformate is 2.1%. The obtained reaction solution was subjected to atmospheric distillation, and 96.3 g of N,N-dimethylformamide dimethyl acetal product was collected, with a purity of 98.1% and a yield of...

Embodiment 2

[0029] Drop into 178.5 grams (1.5mol) chloroform and 162 grams (3mol) sodium methylate in the 2L reactor, methyl alcohol 80 grams, kerosene 455 grams, catalyzer cuprous bromide 3 grams, tetrabutyl ammonium bromide 0.5 grams, close reactor, Turn on the heating, first raise the temperature to about 80°C and react for 2 hours, then slowly raise the temperature to about 120°C and react for 3 hours, cool down to 28°C, press filter, then put the filtrate into the reactor, and feed 180 grams (4mol) of dimethylamine, Close the reactor, turn on the heating to 140-150°C and keep it warm for 2 hours, cool down to below 30°C, take samples for gas phase detection, and deduct the solvent peak: the product purity is 93.5%, chloroform is 3.5%, and trimethyl orthoformate is 1.9%. The obtained reaction solution was subjected to atmospheric distillation, and 150 g of N,N-dimethylformamide dimethyl acetal product was collected, with a purity of 98.4% and a yield of 84%.

Embodiment 3

[0031] The preparation method of N,N-dimethylformamide dimethyl acetal is the same as that of Example 2, except that the solvent used in this example is a mixed solvent of 80 grams of methanol and 455 grams of dearomatized solvent naphtha, to obtain N , 152 grams of N-dimethylformamide dimethyl acetal, with a purity of 98.3% and a yield of 85.2%.

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Abstract

The present invention relates to the field of organic synthesis, in particular to an environmentally friendly preparation method of N,N-dimethylformamide dimethyl acetal, comprising the following steps: sodium methoxide and chloroform generate dimethoxychloromethane under the action of a catalyst; The dimethoxychloromethane obtained in the above steps is reacted with dimethylamine to obtain N,N-dimethylformamide dimethyl acetal. The invention has the advantages of avoiding the use of highly toxic dimethyl sulfate; the sodium chloride produced by the reaction can be sold as a by-product after simple treatment, which can not only reduce the amount of solid waste generated, but also increase the economic benefits of the product.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for preparing N,N-dimethylformamide dimethyl acetal, an important intermediate in organic synthesis. Background technique [0002] N,N-Dimethylformamide dimethyl acetal has a wide range of uses and can be used to synthesize drugs such as zaleplon and imatinib mesylate. It is also a condensing agent in the synthesis of advanced pesticides. In addition, it is used in organic synthesis It has good esterification and dehydration effect and is widely used as a methylation reagent. At present, the demand for N,N-dimethylformamide dimethyl acetal in the market is large and wide. [0003] "Shandong Chemical Industry" 2003 Issue 01, "Preparation of N,N-Dimethylformamide Dimethyl Acetal" adopts the reaction of dimethyl sulfate and N,N-dimethylformamide (DMF) to form an imine complex compound, and then react with sodium methoxide to obtain DMFA with a yield of 40% to 70%. The re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C213/02C07C217/40C07C41/50C07C43/313
CPCC07C41/50C07C213/02C07C217/40C07C43/313
Inventor 李红功曹丽曹媛媛
Owner 常州沃腾化工科技有限公司