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A kind of method for synthesizing 2,6-dimethoxyphenol

A technology of dimethyl carbonate and methanol, applied in 2 fields, can solve the problems of low activity, cumbersome steps, high toxicity, etc., and achieve the effects of high product yield, good safety, and low cost

Active Publication Date: 2019-04-23
贝利科技(重庆)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Disadvantages: 1. The steps are cumbersome and the yield is not high; 2. A large amount of waste acid and waste water are produced; 3. The methylation reagent dimethyl sulfate is highly toxic
[0003] The activity of dimethyl carbonate is lower than that of dimethyl sulfate. At present, there is no literature disclosing the use of dimethyl carbonate to methylate pyrogallic acid to synthesize 2,6-dimethoxyphenol

Method used

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  • A kind of method for synthesizing 2,6-dimethoxyphenol
  • A kind of method for synthesizing 2,6-dimethoxyphenol

Examples

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Effect test

Embodiment 1

[0023] Dissolve 12.6g of pyrogallic acid, 18.9g of dimethyl carbonate, and 0.16g of tetrabutylammonium bromide in 150ml of methanol, pump it into the microreactor after dissolution, flow rate of 2mL / min, reaction pressure of 5MPa, and heat to 120°C, residence time 30min, and the reaction was completed after about 2 hours. After recovering part of the methanol from the reacted feed liquid, 13.3g of 2,6-dimethoxyphenol was obtained by distillation, with a yield of 86% and a purity of 97%.

Embodiment 2

[0025] Dissolve 12.6g of pyrogallic acid, 18.9g of dimethyl carbonate, and 0.16g of tetrabutylammonium bromide in 150ml of methanol, pump it into the microreactor after dissolution, flow rate of 2mL / min, reaction pressure of 5MPa, and heat to 130°C, residence time 30min, and the reaction ends after about 2 hours. After recovering part of the methanol from the reacted feed liquid, distill it to obtain 2,6-dimethoxyphenol 14.1 with a yield of 92% and a purity of 99%.

Embodiment 3

[0027] Dissolve 12.6g of pyrogallic acid, 18.9g of dimethyl carbonate, and 0.16g of tetrabutylammonium bromide in 150ml of methanol, pump it into the microreactor after dissolution, flow rate of 2mL / min, reaction pressure of 5MPa, and heat to 135°C, residence time 30min, and the reaction was completed after about 2 hours. After recovering part of methanol from the reacted liquid, 14.0g of 2,6-dimethoxyphenol was obtained by distillation with a yield of 91% and a purity of 99%.

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Abstract

The invention discloses a method for synthesizing 2,6-dimethoxyphenol. The method includes taking a microreactor as a reaction device and tetrabutylammonium bromide as a catalyst, and enabling pyrogallic acid and dimethyl carbonate to produce the 2,6-dimethoxyphenol by etherification. The method is high in yield and purity, simple in post-treatment and capable of achieving continuous production.

Description

technical field [0001] The invention belongs to the field of fine chemicals, relates to the synthesis of commonly used chemicals, in particular to the industrial synthesis of 2,6-dimethoxyphenol. Background technique [0002] 2,6-dimethoxyphenol is an important chemical and pharmaceutical intermediate. The traditional process uses pyrogallic acid as the raw material, methylated with dimethyl sulfate, and selectively demethylated in two steps. Disadvantages: 1. The steps are cumbersome and the yield is not high; 2. A large amount of waste acid and waste water are produced; 3. The methylation reagent dimethyl sulfate is highly toxic. [0003] The activity of dimethyl carbonate is lower than that of dimethyl sulfate. At present, there is no literature disclosing the use of dimethyl carbonate to methylate pyrogallic acid to synthesize 2,6-dimethoxyphenol. [0004] With the development of science and technology, miniaturization has become an important trend. Compared with conve...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/16C07C43/23
CPCC07C41/16C07C43/23
Inventor 任春和颜廷帅程文峰张雯君杨巧梅徐晓东
Owner 贝利科技(重庆)有限公司
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