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Synthesizing method of beta-menadione

A synthesis method and menadione technology are applied in the preparation of quinone oxide, organic chemistry, etc., and can solve the problems of a large amount of chromium-containing waste water, serious environmental pollution, and high equipment requirements, so as to reduce energy consumption, reduce environmental pollution, and simplify product separation. Effect

Active Publication Date: 2017-06-30
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of β-menaquinone obtained by this method is low; the reaction uses strong acid as the medium, which is highly corrosive and requires high equipment requirements; and a large amount of chromium-containing wastewater will be produced, causing serious environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Weigh 1.4g of β-methylnaphthalene and 3.4g of m-chloroperoxybenzoic acid, dissolve them in 30mL of chloroform to prepare a solution, and ultrasonically react at room temperature for 40min; the reaction solution is filtered and saturated with NaHCO 3 solution, washed with water, anhydrous Na 2 SO 4 After drying, the crude product of β-menaquinone can be obtained by distillation under reduced pressure. The crude product is added with ethanol and activated carbon, heated and dissolved, filtered while hot, the filtrate is cooled and crystallized, and dried by suction filtration to obtain pale yellow crystals, namely β-menaphthalene. Pure quinone, yield 36.5%.

Embodiment 2

[0016] Weigh 1.4g of β-methylnaphthalene and 3.4g of m-chloroperoxybenzoic acid, dissolve in 30mL of chloroform to prepare a solution, and ultrasonically react at 50°C for 40min; the reaction solution is filtered and saturated with NaHCO 3 solution, washed with water, anhydrous Na 2 SO 4 After drying, the crude product of β-menaquinone can be obtained by distillation under reduced pressure. The crude product is added with ethanol and activated carbon, heated and dissolved, filtered while hot, the filtrate is cooled and crystallized, and dried by suction filtration to obtain pale yellow crystals, namely β-menaphthalene. Pure quinone, yield 24.8%.

Embodiment 3

[0018] Weigh 1.4 g of β-methylnaphthalene and 3.4 g of m-chloroperoxybenzoic acid, dissolve them in 30 mL of chloroform to prepare a solution, and perform ultrasonic reaction at room temperature for 1 h; the reaction solution is filtered and saturated with NaHCO 3 solution, washed with water, anhydrous Na 2 SO 4 After drying, the crude product of β-menaquinone can be obtained by distillation under reduced pressure. The crude product is added with ethanol and activated carbon, heated and dissolved, filtered while hot, the filtrate is cooled and crystallized, and dried by suction filtration to obtain pale yellow crystals, namely β-menaphthalene. 3%。 Pure quinone, yield 32.3%.

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Abstract

The invention relates to a synthesizing method of beta-menadione. The synthesizing method comprises the following steps of respectively dissolving a certain amount of beta-methylnaphthalene and metachloroperbenzoic acid into a proper amount of chloroform; performing ultrasonic reaction for a period of time at certain temperature; filtering reaction liquid, washing by saturated NaHCO3 solution and water, and drying by anhydrous Na2SO4; performing reduced pressure distillation to obtain the product of beta-menadione. The synthesizing method has the advantages that the conversion rate of the beta-menadione is 80%; the yield of the beta-menadione is 36%; the reaction time is short, the condition is mild, the product is easily separated, and the like; any catalyst is not used in reaction, and the energy consumption and pollution to environment are decreased.

Description

technical field [0001] The invention relates to a method for synthesizing beta-menaquinone, and belongs to the field of chemical synthesis. Background technique [0002] Beta-menaquinone is vitamin K 3 active ingredient, lack of vitamin K 3 The clotting time of the animals is significantly prolonged, and in severe deficiencies, minor abrasions can cause continuous bleeding and lead to death. In aquaculture and animal husbandry, in order to promote animal growth and prevent diseases, hormones and antibiotics are often added to the feed, resulting in animal vitamin K. 3 of lack. Therefore, vitamin K is added to the feed 3 , to supplement vitamin K in animals 3 It can effectively prevent and treat hemorrhagic diseases of livestock and poultry. In addition, β-menaquinone can be induced to generate active O by flavinase catalysis. 2- , H 2 O 2 and OH - , thereby destroying catalase in tumor cells, producing cytotoxicity, inhibiting or destroying the growth of tumor cell...

Claims

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Application Information

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IPC IPC(8): C07C46/04C07C50/12
CPCC07C46/04C07C50/12
Inventor 黑晓明刘金华魏明志
Owner QILU UNIV OF TECH
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