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The preparation method of p-isopropyl benzoic acid

A technology of isopropyl benzoic acid and citric acid is applied in the direction of carboxylate preparation, organic compound preparation, oxidative preparation of carboxylic acid, etc. It can solve the problems of poor catalytic selectivity, unsatisfactory purity, and high synthesis cost. Achieve excellent catalytic activity, improve purity, and good catalytic activity

Active Publication Date: 2018-07-31
ITIC MEDCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the raw material β-pinene used in this synthesis method has not been purified and contains a small amount of α-pinene, resulting in unsatisfactory purity of the final product. In addition, the palladium used in the dehydrogenation step of dihydrocuminic acid Carbon catalyst is expensive, so the synthesis cost is high, and its catalytic selectivity is not very good, which has a certain impact on the yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Synthesize p-isopropylbenzoic acid according to the following steps:

[0029] (1) Add cerium nitrate and zinc nitrate to citric acid, the molar ratio of cerium nitrate, zinc nitrate and citric acid is 1:1:1, stir for 5 minutes and heat to 80°C, stir until a uniform gel is formed, 80 ℃, 0.8kPa, the gel was rotary evaporated, and then placed in an oven to dry at 180 ℃ for 2 hours to obtain a precursor, and the precursor was calcined in air atmosphere at 600 ℃ for 4 hours to obtain a cerium oxide-zinc oxide composite carrier;

[0030] (2) The cerium oxide-zinc oxide composite carrier that step (1) is obtained is immersed in the chromium nitrate solution that concentration is 0.1mol / L, and the mass ratio of cerium oxide-zinc oxide composite carrier, chromium nitrate solution is 1:50, Stand at room temperature for aging for 24 hours, put it in a vacuum drying oven at 90°C and dry to constant weight, transfer it to a muffle furnace for calcination at 650°C for 4 hours to obta...

Embodiment 2

[0037] Synthesize p-isopropylbenzoic acid according to the following steps:

[0038](1) Add cerium nitrate and zinc nitrate to citric acid, the molar ratio of cerium nitrate, zinc nitrate and citric acid is 1:1:1, stir for 5 minutes and heat to 80°C, stir until a uniform gel is formed, 80 ℃, 0.8kPa, the gel was rotary evaporated, and then placed in an oven to dry at 180 ℃ for 2 hours to obtain a precursor, and the precursor was calcined in air atmosphere at 600 ℃ for 4 hours to obtain a cerium oxide-zinc oxide composite carrier;

[0039] (2) The cerium oxide-zinc oxide composite carrier that step (1) is obtained is immersed in the chromium nitrate solution that concentration is 0.1mol / L, and the mass ratio of cerium oxide-zinc oxide composite carrier, chromium nitrate solution is 1:50, Stand at room temperature for aging for 24 hours, put it in a vacuum drying oven at 90°C and dry to constant weight, transfer it to a muffle furnace for calcination at 650°C for 4 hours to obtai...

Embodiment 3

[0046] Synthesize p-isopropylbenzoic acid according to the following steps:

[0047] (1) Add cerium nitrate and zinc nitrate to citric acid, the molar ratio of cerium nitrate, zinc nitrate and citric acid is 1:1:1, stir for 5 minutes and heat to 80°C, stir until a uniform gel is formed, 80 ℃, 0.8kPa, the gel was rotary evaporated, and then placed in an oven to dry at 180 ℃ for 2 hours to obtain a precursor, and the precursor was calcined in air atmosphere at 600 ℃ for 4 hours to obtain a cerium oxide-zinc oxide composite carrier;

[0048] (2) The cerium oxide-zinc oxide composite carrier that step (1) is obtained is immersed in the chromium nitrate solution that concentration is 0.1mol / L, and the mass ratio of cerium oxide-zinc oxide composite carrier, chromium nitrate solution is 1:50, Stand at room temperature for aging for 24 hours, put it in a vacuum drying oven at 90°C and dry to constant weight, transfer it to a muffle furnace for calcination at 650°C for 4 hours to obta...

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Abstract

The invention provides a method for preparing p-isopropylbenzoic acid. The method includes the following steps that firstly, nitrate cerium and zinc nitrate are prepared through citric acid-nitrate combustion to obtain a cerium oxide-zinc oxide composite carrier; secondly, the cerium oxide-zinc oxide composite carrier is prepared into a composite catalyst through the impregnation method; thirdly, beta-pinene sold in the market is purified with benzenesulfonyl azide to obtain purified beta-pinene; fourthly, the purified beta-pinene is oxidized by potassium permanganate to obtain sodium nopinic acid; fifthly, sodium nopinic acid is acidized with hydrochloric acid to obtain nopinic acid; sixthly, nopinic acid is dehydrated and subjected to ring opening under the action of sulfuric acid to obtain dihydrocumic acid; seventhly, dihydrocumic acid is dehydrogenized under the action of the composite catalyst to obtain p-isopropylbenzoic acid. The yield and the product purity are both high, and preparation cost is low.

Description

technical field [0001] The invention relates to the field of pharmaceutical intermediates, in particular to a preparation method of p-isopropylbenzoic acid. Background technique [0002] p-Isopropyl Benzoic Acid (English name p-Isopropyl Benzoic Acid), also known as 4-isopropyl benzoic acid, 4-isopropyl benzoic acid (4-Isopropyl Benzoic Acid), commonly known as cumic acid, cuminic acid (Cuminic acid) . It is a white powder at room temperature, soluble in water, alcohol and ether, and soluble in concentrated sulfuric acid without decomposing, and re-precipitating crystals after diluting with water. P-cymenic acid is an important fine chemical, which has many uses in polymer materials, oil product improvement, liquid crystal display, medicine, and pesticides. For example, it is used as a raw material for the synthesis of polymer thermistors, used as a preservative, protective agent, mothproof agent and termite-proof agent in the wood industry, and can also be used as a corro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/377C07C63/04B01J23/26
CPCB01J23/002B01J23/26B01J2523/00C07C7/14875C07C51/16C07C51/377B01J2523/27B01J2523/3712B01J2523/67C07C63/04C07C13/40C07C62/04C07C61/22
Inventor 胡海威丁靓闫永平郑辉严辉
Owner ITIC MEDCHEM CO LTD