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Preparation of hydroresorcinol

A technology of cyclohexanedione and resorcinol, applied in the field of chemical synthesis 1, can solve the problems of unfriendly reaction environment, low preparation conversion rate, poor selectivity, etc., and achieves the elimination of recrystallization, reaction conversion rate and selectivity. The effect of improving and reducing the production cost

Active Publication Date: 2005-10-12
ZHEJIANG UNIV OF TECH
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AI Technical Summary

Problems solved by technology

[0005] In order to solve the problems of low conversion rate, poor selectivity, high cost and unfriendly reaction environment in the preparation of 1,3-cyclohexanedione in the prior art, the present invention provides a high conversion rate, good selectivity, low cost, Preparation method of 1,3-cyclohexanedione with mild reaction conditions

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: preparation of modified skeleton nickel catalyst

[0032] 0.15g of ammonium molybdate, 40mL of water and 5g of common skeleton nickel catalyst were sequentially added into a 100mL double-necked round bottom flask, and stirred and impregnated at room temperature for 1h to obtain a Mo-modified skeleton nickel catalyst, wherein Mo accounted for 1.3% of the mass of the catalyst.

Embodiment 2

[0033] Embodiment 2: preparation of modified skeleton nickel catalyst

[0034] 0.3g of sodium molybdate, 30mL of water and 5g of common skeleton nickel catalyst were sequentially added into a 50mL double-necked round-bottomed flask, stirred and impregnated at room temperature for 2h to obtain a Mo-modified skeleton nickel catalyst, in which Mo accounted for 2.1% of the mass of the catalyst.

Embodiment 3

[0035] Embodiment 3: the preparation of 1,3-cyclohexanedione

[0036] In a 300mL double-necked round bottom flask, add 130mL of water and 35g of potassium hydroxide, stir until the potassium hydroxide is completely dissolved, then add 55g of resorcinol, and stir for 1h. Transfer the obtained resorcinol potassium salt solution to a 0.5L pressure reactor, add 0.5g of the modified skeleton nickel catalyst obtained in Example 1, seal the reactor, replace the air in the reactor with nitrogen for three times, and then replace it with hydrogen Three times, pass hydrogen to 1.5MPa, raise the temperature to 120°C, stir the reaction, when the pressure drops to 0.5MPa, then pass hydrogen to 1.5MPa, and react for 80min until no hydrogen is absorbed. Cool the reaction liquid to below 50°C, discharge the material, remove the catalyst by filtration, transfer the filtrate to a 500 mL two-necked round bottom flask, add 60 mL of concentrated hydrochloric acid with a concentration of 37% dropwis...

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PUM

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Abstract

Production of hydroresorcinol is carried out by taking resorcinol and inorganic alkali with amount ratio 1:1-1.5, neutralizing to be salt, hydrogenating reducing the salt under catalysis of modified skeletal nickel catalyst with molybdenum content 0.5-5%, 0.5-3Mpa and 50-150deg.C, hydrogenated and reduced product acidizing and re-arranging reacting with Bronsted acid at room-temperature, and obtaining hydroresorcinol. It achieves lower cost, higher percent conversion and selectivity.

Description

(1) Technical field [0001] The invention relates to a method for chemically synthesizing 1,3-cyclohexanedione, which belongs to the category of organic synthetic chemistry [0002] technology field. (2) Background technology [0003] 1,3-Cyclohexanedione is an important intermediate in the synthesis of carvedilol, a special drug that protects cardiovascular and cerebrovascular diseases, and treats high blood pressure, and anthrandansetone, an antiemetic drug. It is also an important intermediate for the synthesis of herbicides sulcotrione and An essential intermediate of mesotrione. [0004] There are two main methods for synthesizing 1,3-cyclohexanedione, that is, using sodium alkoxide as a condensing agent, amides, etc. as a reaction medium, and cyclizing γ-acetylbutyrate to synthesize 1,3-cyclohexanedione The condensation method of ketone and the reduction method of synthesizing 1,3-cyclohexanedione with resorcinol as the starting material through neutralization, hydrog...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/41C07C45/52C07C49/403
Inventor 徐振元胡智燕许丹倩
Owner ZHEJIANG UNIV OF TECH
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