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Method for preparing 3,4-dimethoxytoluene by using monobromomethane-containing waste gas as raw material

A technology of dimethoxytoluene and methyl bromide, applied in ether preparation, organic chemistry, etc., can solve the problems of ineffective production, uneconomical, high recycling costs, and achieve good environmental and economic benefits, good market and application Prospect, selectivity and high yield effect

Inactive Publication Date: 2014-03-26
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of these reactions require catalysts, and the yield varies from 10% to 90%, accompanied by the generation of by-products, and the selectivity is not high. Therefore, this approach cannot effectively produce 3,4-dimethoxytoluene
(3) Using 4-methyl catechol or 4-formyl catechol as raw material and Me 2 SO 4 The reaction generates 3,4-dimethoxytoluene, and the yield of this type of reaction is higher, and the reaction steps are less, but due to Me 2 SO 4 Very easy to hydrolyze, the reaction must be carried out in an organic solvent, so it is difficult to separate the product
And the latter requires the participation of a catalyst, which increases the production cost
(4) It is also reported that 3,4-dimethoxytoluene is synthesized from p-cresol or 1,2-dimethoxybenzene as a raw material, but these reaction steps are more and the reaction time is long, which is not suitable for 3,4- Industrial production of dimethoxytoluene
If the exhaust gas is condensed to recover methyl bromide, the recovery cost is high and it is not economical

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Weigh 8.28g (0.06mol) of 4-methylguaiacol into a 100ml two-necked flask, add 30ml of 2M KOH solution, slowly heat up to 100°C under stirring, and introduce The industrial waste gas in the reaction until the reaction is complete, the isolated yield of 3,4-dimethoxytoluene is 96.3%.

Embodiment 2

[0017] Weigh 8.28g (0.06mol) 4-methylguaiacol in a 100ml two-necked flask, add 30ml 2M NaOH solution and 0.137g catalyst (CH 3 ) 4 In NBr, the temperature was slowly raised to 120° C. under stirring, and the industrial waste gas from the synthesis process of methyl catechol was introduced until the reaction was complete. The isolated yield of 3,4-dimethoxytoluene was 99.2%.

Embodiment 3

[0019] Weigh 8.28g (0.06mol) 4-methylguaiacol in a 100ml two-necked flask, add 30ml 2M NaOH solution and 0.30g (C 4 h 9 ) 4 In NBr, the temperature was slowly raised to 80° C. under stirring, and the industrial waste gas from the synthesis process of methyl catechol was introduced until the reaction was complete. The isolated yield of 3,4-dimethoxytoluene was 99.1%.

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Abstract

The invention provides a method for preparing 3,4-dimethoxytoluene by using monobromomethane-containing waste gas as a raw material, which comprises the following steps of: alkalifying 4-methyl guaiacol by using aqueous solution of inorganic base; and heating solution of the alkalified 4-methyl guaiacol until the temperature is between 60 and 150 DEG C, introducing the monobromomethane-containing waste gas, and after a reaction is finished, cooling reaction solution and separating directly to obtain the 3,4-dimethoxytoluene. A small amount of catalyst is added into the reaction solution, so that the reaction speed and the selectivity of a target product can be improved. The method provided by the invention can be used for recycling monobromomethane-containing industrial waste gas with high 3,4-dimethoxytoluene selectivity and yield. In addition, the method is simple and low in cost and has an excellent application prospect.

Description

【Technical field】 [0001] The invention relates to the fields of fine chemical industry and organic synthesis, and more specifically relates to a method for preparing 3,4-dimethoxytoluene by using waste gas containing bromomethane as a raw material. 【Background technique】 [0002] 3,4-Dimethoxytoluene (3,4-Dimethoxytoluene), also known as 1,2-dimethoxy-4-methylbenzene, is an important intermediate in the synthesis of perfumes and pharmaceuticals, and has a large market demand. At present, the synthesis of 3,4-dimethoxytoluene mainly has the following approaches: (1) It is obtained by decomposing complex compounds containing 3,4-dimethoxytoluene structure, wherein 3,4-dimethoxytoluene is used as a by-product product produced. Such synthesis method, the yield of 3,4-dimethoxytoluene is very low, and the product is complex, difficult to separate, and cannot efficiently produce 3,4-dimethoxytoluene. (2) The hydrogen on the 3,4-dimethoxytoluene methyl group is replaced by a halo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/205C07C41/01
Inventor 尹双凤欧阳强
Owner HUNAN UNIV
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