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Method for synthesizing R-(+)-2-(4-hydroxyphenoxy)propionic acid through gas phase catalysis

A hydroxyphenoxy, gas-phase technology, applied in the field of R--2-propionic acid preparation, to achieve the effect of less equipment corrosion, good stability and strong acidity

Active Publication Date: 2020-05-22
JIANGSU SANJILI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to address the problems faced by the current synthesis of R-(+)-2-(4-hydroxyphenoxy)propionic acid, and propose a loaded heteropolyacid as a catalyst to catalyze hydroquinone and D-lactic acid A new process for preparing R-(+)-2-(4-hydroxyphenoxy)propionic acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1 Preparation of loaded heteropolyacid, wherein the molar ratio of P:W:V is 1:8:5.

[0023] (1) Add 37.5g of NH 4 VO 3 and 23.8 g of Na 2 HPO 4 12H 2 O was made into 1000mL and 300mL aqueous solutions respectively, adjusted to pH=6 with glacial acetic acid, and 174.8g of Na 2 WO 4 2H 2 O was dissolved in water to form a 330mL aqueous solution, adjusted to PH=4 with 8mol / L sulfuric acid, and Na 2 HPO 4 The solution was gradually and slowly added to NH 4 VO 3 , fully stirred, and then adjusted to PH = 3 with 8mol / L sulfuric acid, continued to stir and heat in a boiling water bath for 1h, and then added dropwise Na 2 WO 4 Aqueous solution, after dripping, continue stirring and heating until the solution volume is 1 / 5 of the original volume, filter the precipitate, leave the filtrate for 24 hours, and recrystallize twice after crystallization to prepare (NH 4 ) 6 HPV 4 W 8 o 40 14H 2 O heteropoly acid 150g.

[0024] (2) Take 100g of silica gel and ...

Embodiment 2

[0027] Put 50 g of the catalyst prepared in Example 1 into a stainless steel fixed-bed reactor with an inner diameter of 20 mm, control the gasification temperature at 280° C., and the reaction temperature at 240° C., 62.5 g of hydroquinone and 40.9 g of D-lactic acid were evenly added to the In the gasification chamber, the nitrogen flow rate is controlled at 100mL / min at the same time, and the gasified mixture is brought into the fixed-bed reactor with nitrogen as the carrier gas, and R-(+)-2 is prepared by reaction under the condition of catalyst. -(4-Hydroxyphenoxy)propanoic acid. Through liquid chromatography analysis product, the retention time of hydroquinone raw material peak is 1.965min, and the retention time of R-(+)-2-(4-hydroxyphenoxy group) propionic acid product peak is 6.065min, and hydroquinone The effective conversion rate of phenol is high, and the calculated selectivity of R-(+)-2-(4-hydroxyphenoxy)propionic acid is 80.5%.

Embodiment 3

[0029]Put 50 g of the catalyst prepared in Example 1 into a stainless steel fixed-bed reactor with an inner diameter of 20 mm, control the gasification temperature to 280° C., and the reaction temperature to 250° C., 62.5 g of hydroquinone and 46.0 g of D-lactic acid were evenly added to the In the gasification chamber, the nitrogen flow rate is controlled at 110mL / min at the same time, and the gasified mixture is brought into the fixed-bed reactor with nitrogen as the carrier gas, and the R-(+)-2 -(4-Hydroxyphenoxy)propanoic acid. The product was analyzed by liquid chromatography, the peak time was unchanged, the effective conversion rate of hydroquinone was high, and the selectivity of R-(+)-2-(4-hydroxyphenoxy)propionic acid was calculated to be 80.0%.

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Abstract

The invention discloses a method for synthesizing R-(+)-2-(4-hydroxyphenoxy)propionic acid through gas phase catalysis, and belongs to the field of organic synthesis. Hydroquinone and D-lactic acid are used as raw materials, and nitrogen is used as a carrier gas. The hydroquinone and the D-lactic acid are completely gasified and then enter a fixed bed reactor, and the R-(+)-2-(4-hydroxyphenoxy)propionic acid is continuously synthesized in a gas phase under the catalysis of a supported heteropolyacid catalyst. The method has the advantages of mild reaction conditions, simple reaction process, high effective conversion rate of hydroquinone and high selectivity of the R-(+)-2-(4-hydroxyphenoxy) propionic acid, and is completely suitable for industrial production, and the self-made supported heteropolyacid solid catalyst has excellent catalytic activity, strong acidity, good stability and no pollution to the environment, and is a green catalyst.

Description

technical field [0001] The present invention relates to a kind of preparation method of R-(+)-2-(4-hydroxyphenoxy group) propionic acid, specifically under the gas phase condition heteropoly acid catalyzes hydroquinone and D-lactic acid to prepare R-( +)-2-(4-hydroxyphenoxy)propionic acid method. Background technique [0002] R-(+)-2-(4-hydroxyphenoxy)propionic acid is mainly used for the synthesis of R-(+)-2-(4-hydroxyphenoxy)propionic acid methyl ester, R-(+)-2 -(4-hydroxyphenoxy) ethyl propionate, R-(+)-2-(4-hydroxyphenoxy) butyl propionate and other special intermediates and their downstream products quizalofop-p Aryloxyphenoxypropionate herbicides such as fluazifop-methyl, high-efficiency fluroxyfop, clodinafop-propargyl, etc. Aryloxyphenoxypropionate herbicides are a class of herbicides that can effectively control grass weeds. They have the characteristics of high efficiency, low toxicity, and safety to subsequent crops. They are also a class of herbicides that deve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/367C07C59/68B01J27/24B01J27/199B01J31/18
CPCC07C51/367B01J27/199B01J27/24C07B2200/07C07C59/68
Inventor 杨世刚唐伟伏建波张磊董卫星
Owner JIANGSU SANJILI CHEM
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