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A kind of preparation method of 3,7-diethylnonane-4,6-dione

A technology of ethyl nonane and diketone, which is applied in the field of organic chemical synthesis, can solve the problems of harsh reaction conditions and low yield, and achieve the effects of low cost, safe yield and convenient operation

Active Publication Date: 2021-08-31
ASTATECH CHENGDU BIOPHARM CORP
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method has simple steps, the yield is low and the reaction conditions are harsh.

Method used

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  • A kind of preparation method of 3,7-diethylnonane-4,6-dione
  • A kind of preparation method of 3,7-diethylnonane-4,6-dione
  • A kind of preparation method of 3,7-diethylnonane-4,6-dione

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Experimental program
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Effect test

Embodiment 1

[0026] S1. Ethylmagnesium bromide (700ml, 5.5eq) was added to a three-necked flask, and a tetrahydrofuran (100g) solution containing dimethyl isophthalate (50g, 1.0eq) was added dropwise at 0°C. After the dropwise addition, the temperature was naturally raised to 25°C, and the system reacted for 2.5-4 hours. After the reaction, the reaction system was slowly poured into an aqueous ammonium chloride solution, and the product 2-3 was extracted with ethyl acetate (1000g), and the organic phase was concentrated to dryness. The residue was recrystallized from n-heptane to obtain 3,3'-(1,3-phenylene)bis(3-pentanol) with a yield of 76.8%.

[0027] S2. Dissolve the above 3,3'-(1,3-phenylene)bis(3-pentanol) (10g, 1.0eq) in acetic acid (50g), pour it into an autoclave, add 10% Pd / C (0.5g), replace with hydrogen, make the internal pressure 1.0-2.0MPa, heat the external bath to 100°C, react for 16h, after the reaction is completed, cool, filter, wash the filter cake with petroleum ether, ...

Embodiment 2

[0031] S1. Ethylmagnesium bromide (420ml, 5.5eq) was added to a three-necked flask, and a solution of tetrahydrofuran (50g) containing dimethyl isophthalate (30g, 1.0eq) was added dropwise at 0°C. After the dropwise addition, the temperature was naturally raised to 25° C., and the system reacted for 2.5-4 hours. After the reaction, the reaction system was slowly poured into an aqueous ammonium chloride solution, and the product 2-3 was extracted with ethyl acetate (600 g), and the organic phase was concentrated to dryness. The residue was recrystallized from n-heptane to obtain 3,3'-(1,3-phenylene)bis(3-pentanol) with a yield of 74.2%.

[0032] S2. Dissolve the above 3,3'-(1,3-phenylene)bis(3-pentanol) (30g, 1.0eq) in acetic acid (250g), pour it into an autoclave, add 10% Pd / C (5.5g), replace with hydrogen, make the internal pressure 1.5-2.0MPa, heat the external bath to 100°C, react for 16h, after the reaction is completed, cool, filter, wash the filter cake with petroleum et...

Embodiment 3

[0036]S1. Ethylmagnesium bromide (700ml, 5.5eq) was added to a three-necked flask, and a tetrahydrofuran (100g) solution containing dimethyl isophthalate (50g, 1.0eq) was added dropwise at 0°C. After the dropwise addition, the temperature was naturally raised to 25°C, and the system reacted for 2.5-4 hours. After the reaction, the reaction system was slowly poured into an aqueous ammonium chloride solution, and the product 2-3 was extracted with ethyl acetate (1000g), and the organic phase was concentrated to dryness. The residue was recrystallized from n-heptane to obtain 3,3'-(1,3-phenylene)bis(3-pentanol) with a yield of 76.8%.

[0037] S2. Dissolve the above 3,3'-(1,3-phenylene)bis(3-pentanol) (30g, 1.0eq) in acetic acid (200g), pour it into an autoclave, add 10% Pd / C (4.5g), replace with hydrogen, make the internal pressure 1.3-1.6MPa, heat the external bath to 100°C, react for 18h, after the reaction is completed, cool, filter, wash the filter cake with petroleum ether, ...

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Abstract

The invention discloses a preparation method of 3,7-diethylnonane-4,6-dione, which belongs to the field of chemical synthesis. "A preparation method of 3,7-diethylnonane-4,6-dione" of the present invention uses low-cost dimethyl isophthalate as a raw material, through elimination, addition, catalytic hydrogenation reaction, Birch The preparation of 3,7-diethylnonane-4,6 diketone by four-step reaction of reduction and ozonation, the method is low in cost, short in synthesis process, mild in reaction conditions, convenient in operation, safe and high in yield, suitable for large Large-scale industrial production.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to a preparation method of 3,7-diethylnonane-4,6-dione. Background technique [0002] 3,7-diethylnonane-4,6-dione is widely used as a coating for electronic components, but the synthesis methods reported at home and abroad have certain defects. [0003] In 1951, Eugene H.Man et al. reported a synthetic 3,7-diethyl The method of diethylnonane-4,6-dione, the method is to adopt 2-ethylbutyric acid as starting material, and obtain 3,7-diethylnonane-4,6-dione through six-step reaction . Although this method is easy to operate in each step, it has many process steps and intermediate 6 is difficult to purify due to its low boiling point; the last step reaction itself is more complicated, the phenol produced by the reaction is not easy to remove, and the final product is extremely difficult to purify and has a low yield. The reaction formula is as follows: [0004] [0005] ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/12C07C45/40C07C5/11C07C13/23C07C1/22C07C15/02C07C29/36C07C33/26
CPCC07C1/22C07C5/11C07C29/36C07C45/40C07C2523/04C07C2523/44C07C2601/16C07C33/26C07C15/02C07C13/23C07C49/12
Inventor 陈孝刚庄明晨柯东磊罗建业郭鹏
Owner ASTATECH CHENGDU BIOPHARM CORP
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