A kind of synthetic method of oxyisophorone

A technology of oxyisophorone and synthesis method, which is applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problems of dangerous operating conditions and high cost of reaction process, and achieve less discharge of three wastes, Process-friendly, high-yield results

Active Publication Date: 2020-04-28
SHANGYU NHU BIOCHEM IND +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the method has a high yield, the reaction process cost is high, and the operating conditions are very dangerous

Method used

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  • A kind of synthetic method of oxyisophorone
  • A kind of synthetic method of oxyisophorone
  • A kind of synthetic method of oxyisophorone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] 1) Add industrial product HIP equivalent to 30.0g (0.1945mol) of pure HIP, 60.0g toluene into a four-neck flask, heat up to 80°C under 300rpm stirring condition, blow air through bubbling method, and add 10.8g p-benzoquinone dropwise (0.10mol) + toluene 30.0g mixed solution, after the dropwise addition, keep the temperature at 80±10°C, continue to ventilate the air, react for 2-5 hours, GC detects that the HIP residue < 0.1% stops the reaction;

[0050] 2) Add aqueous sodium thiosulfate solution (100ml, mass concentration 15-20%) to the reaction solution in step 1) and stir for 30min, then add (in two times, 50mL each time) 5% sodium hydroxide solution for washing, after layering , the aqueous phase is an alkali washing solution, and the organic phase is washed with 30ml of water as a reaction solution,

[0051] 3) In a four-neck flask, stir and feed in air at 70-80°C, react for 2-3 hours, add 30g of toluene and stir for 10min, cool down to room temperature, let stand, ...

Embodiment 2

[0054] 1) Add the industrial product HIP (0.2075mol) equivalent to 32.0g of pure HIP, 60.0g toluene, and heat up to 80°C under 300rpm stirring conditions in a four-necked flask, and add trimethylbenzoquinone dropwise with air by bubbling method 15.0g (0.10mol) + toluene 45.0g mixed solution, after the dropwise addition, keep the temperature at 80±10°C, continue to ventilate the air, react for 3-5 hours, GC detects that the HIP residue < 0.1% stops the reaction;

[0055] 2) Add aqueous sodium thiosulfate solution (100ml, mass concentration 15-20%) to the reaction solution in step 1) and stir for 30min, then add (twice, 70ml each) 5% sodium hydroxide solution for washing, after layering , the aqueous phase is an alkali washing solution, and the organic phase is used as a reaction solution after washing with 50ml of water;

[0056] 3) In a four-neck flask, stir and feed in air at 70-80°C, react for 2-3 hours, add 35g of toluene and stir for 10 minutes, cool down to room temperatu...

Embodiment 3

[0059] 1) Add industrial product HIP equivalent to 35.0g (0.2270mol) of pure HIP, 65.0g p-xylene into a four-necked flask, heat up to 100°C under 300rpm stirring condition, air-bubble method, drop trimethyl Benzoquinone 20.0g (0.1333mol) + p-xylene 45.0g mixed solution, after the dropwise addition, keep the temperature at 100±10°C, continue to ventilate the air, react for 3-5 hours, GC detects that the HIP residue < 0.1% stops the reaction,

[0060] 2) Add aqueous sodium thiosulfate solution (100ml, mass concentration 15-20%) to the reaction solution in step 1) and stir for 30min, then add (twice, 70mL each) 5% sodium hydroxide solution for washing, after layering , the aqueous phase is an alkali washing solution, and the organic phase is washed with 50ml of water as a reaction solution,

[0061] 3) In a four-neck flask, stir and feed in air at 70-80°C, react for 2-3 hours, add 35g of p-xylene and stir for 10min, drop to room temperature, let stand, and separate the organic ph...

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Abstract

Provided is a method for synthesizing keto-isophorone. The method comprising: using 3,5,5-trimethyl-4-hydroxy-2-cyclohexene-1-one (HIP) as a raw material; using a benzoquinone compound (II) as an oxidizing agent and a catalyst; introducing oxygen or air; oxidizing an inert solvent to generate a keto-isophorone (KIP) and a hydroquinone compound (III);

Description

technical field [0001] The invention relates to the field of fine chemical industry, in particular to an oxoisophor with 3,5,5-trimethyl-4-hydroxy-2-cyclohexen-1-one (hereinafter referred to as HIP) as the starting material Synthesis of ketones. Background technique [0002] Oxyisophorone (2,6,6-trimethyl-2-cyclohexene-1,4-dione, 4-Ketoisophorone, referred to as KIP, CAS: 1125-21-9) is a synthetic biotin Key intermediate, its structural formula is as follows: [0003] [0004] The preparation method of oxyisophorone is generally that β-isophorone is used as a raw material, and then oxidized into oxoisophorone. Its existing routine synthetic route is as follows:, [0005] [0006] The above route uses β-isophorone (3,5,5-trimethylcyclohex-3-en-1-one, β-Isophorone, referred to as β-IP, CAS: 78-59-1) as raw material, Obtained by oxidation, in the reaction, oxoisophorone (KIP) as the product and 3,5,5-trimethyl-4-hydroxyl-2-cyclohexen-1-one ( HIP) and 3-formyl-5,5-dim...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/37C07C49/603C07C45/78
CPCC07C45/37C07C45/78C07C49/603
Inventor 杭姣夏小忠李伟明刘祥洪曾庆宇毛建拥乔胜超
Owner SHANGYU NHU BIOCHEM IND
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