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Bimetallic composite catalyst for preparing afloqualone and method for preparing afloqualone

A technology of bimetallic catalysts and composite catalysts, applied in the direction of metal/metal oxide/metal hydroxide catalysts, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of low product purity and poor chemical selectivity, and achieve simple operation , Improve the purity and reduce the content of impurities

Active Publication Date: 2015-06-03
HANGZHOU DOEASY PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the shortcomings of low product purity and poor chemical selectivity in the existing fluoroquinone preparation process, the present invention discloses a bimetallic composite catalyst for preparing fluoroquinone, and also discloses a preparation method of fluoroquinone; in the preparation process Strong chemical selectivity, convenient preparation, simple conditions, safe and reliable, suitable for industrial production

Method used

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  • Bimetallic composite catalyst for preparing afloqualone and method for preparing afloqualone

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Embodiment 1

[0035] A bimetallic composite catalyst for preparing fluoroquinone comprises a ruthenium-palladium catalyst and activated carbon, wherein the mass ratio of metal ruthenium to metal palladium is 1:5, and the mass of the ruthenium-palladium catalyst is 1% of the mass of the activated carbon.

[0036] The preparation method of fluoroquinone, in the process of preparing fluoroquinone, the above catalyst for preparing fluoroquinone is used as catalyst, comprising the following steps:

[0037] A. Add 31.3 grams of 6-nitro-2-(fluoromethyl)-3-(2-methylphenyl)-4-(3H)-1,3-naphthyridine, containing An acid-containing alcohol solution with an acid content of 0.1N and a bimetallic composite catalyst are reacted at a hydrogen pressure of 0.02MPa and a temperature of 0°C. The reaction is followed by liquid chromatography. When the raw materials are completely reacted, the reaction ends. It takes 2 hours to obtain Ruthenium palladium catalyst and filtrate.

[0038] B. Wash the ruthenium pall...

Embodiment 2

[0046] A bimetallic composite catalyst for preparing fluoroquinone, comprising a ruthenium-palladium catalyst and activated carbon, wherein the mass ratio of metal ruthenium to metal palladium is 1:10; the mass of the ruthenium-palladium catalyst is 5% of the mass of the activated carbon.

[0047] The preparation method of fluoroquinone, in the process of preparing fluoroquinone, the above catalyst for preparing fluoroquinone is used as catalyst, comprising the following steps:

[0048] A. Add 6-nitro-2-(fluoromethyl)-3-(2-methylphenyl)-4-(3H)-1,3-phthalazinone, acid content to the hydrogenation unit It is a 0.1N 0.3N acid-containing alcohol-ester mixed solution and a bimetallic composite catalyst. The hydrogen pressure is 0.02MPa and the temperature is 5°C. The reaction is followed by liquid chromatography. When the raw materials are completely reacted, the reaction ends. Hours, filtered to obtain ruthenium palladium catalyst and filtrate.

[0049] B. Wash the ruthenium pall...

Embodiment 3

[0056] A bimetallic composite catalyst for preparing fluoroquinone, comprising ruthenium palladium catalyst and alumina, the mass ratio of metal ruthenium and metal palladium is 1:20; the mass ratio of ruthenium palladium catalyst is 7% of the mass of alumina;

[0057] The preparation method of fluoroquinone, in the process of preparing fluoroquinone, the above catalyst for preparing fluoroquinone is used as catalyst, comprising the following steps:

[0058] A. Add 6-nitro-2-(fluoromethyl)-3-(2-methylphenyl)-4-(3H)-1,3-phthalazinone, acid content to the hydrogenation unit It is a 0.3N acid-containing alcohol-ester mixed solution and a bimetallic composite catalyst. The hydrogen pressure is 0.4MPa and the temperature is 70°C. The reaction is followed by liquid chromatography. When the raw materials are completely reacted, the reaction ends. The total time is 20 hours. The ruthenium palladium catalyst and the filtrate were obtained by filtration.

[0059] B. Wash the ruthenium ...

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Abstract

The invention relates to the field of organic synthesis and discloses a bimetallic composite catalyst for preparing afloqualone. The bimetallic composite catalyst comprises a bimetallic catalyst and a carrier, wherein the bimetallic catalyst is a ruthenium-palladium catalyst or a palladium-platinum catalyst or a palladium-ruthenium catalyst; the carrier is activated carbon or alumina or zeolite. The bimetallic composite catalyst is adopted in the process of preparing the afloqualone, catalytic hydrogenation is performed at low pressure, and the yield and reaction selectivity are effectively improved. The invention also relates to a method for preparing the afloqualone. The method comprises the following steps: with 6-nitro-2-(fluoromethyl)-3-(2-methylphenyl)-4-(3H)-1,3-phthalazinone as a substrate and the bimetallic composite catalyst for preparing the afloqualone as a catalyst, reducing, filtering, regulating a PH value and recrystallizing to prepare the afloqualone. The preparation method is high in chemical selectivity and accords with a green chemistry idea, and the prepared product is high in purity and has wide application prospects.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a bimetallic composite catalyst for preparing fluoroquinone, and also relates to a preparation method of fluoroquinone. Background technique [0002] Fluoroquinone is a muscle relaxant, the drug acts on a wider area of ​​the upper spinal cord center, and then relieves the hypertonic state of the muscles. Fluoroquinone is a relaxant that has a good effect on muscle spasm in the face and neck. It has been clinically used for more than 20 years and has achieved good medical results. For example, it is applied to the following symptoms: cerebrovascular disorders, cerebral palsy, Spastic spinal cord palsy, spinal cord vascular disorders, ossification of the posterior longitudinal ligament, multiple sclerosis, amyotrophic lateral sclerosis, spinocerebellar degeneration, traumatic sequelae (spinal cord injury, head trauma), postoperative sequelae (including brain, spinal cord tumors) a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/46B01J23/44B01J29/00C07D239/91
Inventor 边高峰刘西敬
Owner HANGZHOU DOEASY PHARMA
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