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Method for preparing 4-butyl resorcinol

A technology of butylresorcinol and resorcinol, which is applied in the field of preparing 4-butylresorcinol, can solve the problems of butyryl chloride or n-butyric acid with strong odor, difficult operation, and high reduction reaction temperature of Huang Minglong. Achieve the effects of reducing raw materials and operating costs, facilitating operation, and facilitating large-scale production

Inactive Publication Date: 2020-03-24
抚顺东科新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The butyryl chloride or n-butyric acid used in this method has a big smell, and the reduction reaction temperature of Huang Minglong is high, so it is not easy to operate

Method used

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  • Method for preparing 4-butyl resorcinol
  • Method for preparing 4-butyl resorcinol
  • Method for preparing 4-butyl resorcinol

Examples

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Embodiment 1

[0035] ① Preparation of 2.4-dihydroxybenzaldehyde: under argon protection, add 200 ml of anhydrous N,N-dimethylformamide and 50 grams of resorcinol to a 500 ml reaction bottle, and cool down to 0-5 degrees , slowly add 83.55 grams of phosphorus oxychloride dropwise, after the dropwise addition, heat up to 60 degrees to react for 8 hours, concentrate and recover the solvent under reduced pressure, pour the residue into 300 grams of ice water, add sodium hydroxide to adjust to PH=7, After stirring for 30 minutes, adjust the pH to 3 with dilute hydrochloric acid, filter, and dry the filter cake to obtain 58 g of off-white solid 2.4-dihydroxybenzaldehyde with a yield of 93%.

[0036] ②Preparation of 2,4-dihydroxybenzylideneacetone: Add 58 grams of 2.4-dihydroxybenzaldehyde and 200 milliliters of acetone into a 500 milliliter reaction bottle, slowly add 100 milliliters of 20% sodium hydroxide solution dropwise below 10 degrees, After the dropwise addition, react at 35°C for 10 hour...

Embodiment 2

[0039] ① Preparation of 2.4-dihydroxybenzaldehyde: under argon protection, add 200 ml of anhydrous N,N-dimethylformamide and 50 grams of resorcinol to a 500 ml reaction bottle, and cool down to 0-5 degrees , slowly add 83.55 grams of phosphorus oxychloride dropwise, after the dropwise addition, heat up to 60 degrees to react for 8 hours, concentrate and recover the solvent under reduced pressure, pour the residue into 300 grams of ice water, add sodium hydroxide to adjust to PH=7, After stirring for 30 minutes, adjust the pH to 3 with dilute hydrochloric acid, filter, and dry the filter cake to obtain 58 g of off-white solid 2.4-dihydroxybenzaldehyde with a yield of 93%.

[0040] ②Preparation of 2,4-dihydroxybenzylidene acetone: Add 58 grams of 2.4-dihydroxybenzaldehyde and 200 ml of acetone into a 500 ml reaction bottle, slowly add 100 ml of 20% potassium hydroxide solution dropwise below 10 degrees After the dropwise addition, react at 35°C for 8 hours, lower the temperature...

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Abstract

The invention discloses a method for preparing 4-butyl resorcinol. The method comprises the following steps: (1) preparing 2, 4-dihydroxy benzaldehyde; (2) preparing 2, 4-dihydroxy benzylidene acetone; and (3) preparing the 4-butyl resorcinol. The method has the advantages as follows: firstly, raw materials and reagents used in the method are lower in toxicity, safer, cheaper, easier to obtain andconvenient to store, and the raw material cost and operation cost are greatly reduced; secondly, the method has few reaction steps, is convenient to operate, and is easier for large-scale production;and thirdly, high-toxicity three wastes are not generated, environmental pollution is reduced, and the ecological environment is protected. Meanwhile, the yield of the prepared product is high and can reach 90% or above.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for preparing 4-butylresorcinol. Background technique [0002] 4-Butylresorcinol, also known as 4-butylresorcinol, molecular formula: C 10 h 14 o 2 , molecular weight: 166.22; It is white or off-white powder solid, and it is widely used, especially in the field of cosmetics, 4-butyl resorcinol can be used as whitening agent, antioxidant and preservative; Its characteristics are mainly: 1. Melanosis, chloasma and freckles; 2. Anti-ultraviolet rays; 3. Fast penetration, quickly reaching the deep layer of the skin; 4. High safety and low allergenicity. With the continuous expansion of its use, the market demand is also increasing. The main method for synthesizing 4-butyl resorcinol at present is as follows: [0003] Method one: take resorcinol as raw material, take Lewis acid (aluminum trichloride, zinc chloride etc.) as catalyst, carry out Fried...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/00C07C39/08
CPCC07C37/003C07C45/74C07C45/455
Inventor 刘勇闫纪晨张寞然胡玉珊
Owner 抚顺东科新能源科技有限公司