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Method for promoting beta-menadione production through ultrasonic waves

A technology of menaquinone and ultrasonic wave is applied in the field of promoting the production of β-menaquinone by ultrasonic wave, which can solve the problems of low molar yield and the like

Active Publication Date: 2014-01-01
SICHUAN YINHE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reaction temperature of the prior art is usually 45-60°C, at this time the reaction mass yield is usually lower than 70%, that is, the molar yield is lower than 60%

Method used

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  • Method for promoting beta-menadione production through ultrasonic waves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Prepare the oxidation solution, which contains 390g / L of sodium rubidin and 550g / L of sulfuric acid in the oxidation solution. Weigh 19.19g of β-methylnaphthalene into a 500mL beaker, add 0.2g of tetrabutylammonium bromide as a phase transfer agent, add 80mL of water, stir and ultrasonicate, the ultrasonic power density is 0.75W / L. At 42°C, 285 mL of the above oxidizing solution was slowly added dropwise into the beaker, and the reaction time was 90 minutes. Filter, wash with water, and dry to obtain 15.13 g of β-menadione. The purity of the product β-menaquinone is 95.34%, and the molar yield is 62.07%. The resulting β-menaquinone crystal had a melting point of 105.6°C.

Embodiment 3

[0045] Prepare the oxidation solution, which contains 360g / L of sodium rubidin and 620g / L of sulfuric acid in the oxidation solution. Weigh 86.54g of β-methylnaphthalene into a 2000mL beaker, add 1.2g of tetrabutylammonium bromide as a phase transfer catalyst, add 240mL of water, stir and ultrasonicate, the ultrasonic power density is 3W / L. At 40°C, 1280 mL of the above oxidizing solution was slowly added dropwise into the beaker, and the reaction time was 90 minutes. Filter, wash with water, and dry to obtain 68.13 g of β-menadione, the product β-menaquinone content is 94.18%, and the molar yield is 61.22%. The resulting β-menaquinone crystal had a melting point of 105.4°C.

Embodiment 5

[0050] Prepare the oxidation solution, which contains 390g / L of sodium rubidin and 550g / L of sulfuric acid in the oxidation solution. Weigh 19.19g of β-methylnaphthalene into a 500mL beaker, add 0.2g of tetrabutylammonium bromide as a phase transfer catalyst, add 80mL of water, stir and ultrasonicate, the ultrasonic power density is 1.3W / L. At 42°C, 285 mL of the above oxidizing solution was slowly added dropwise into the beaker, and the reaction time was 90 minutes. Filter, wash with water, and dry to obtain 14.97 g of β-menadione. The product β-menaquinone has a purity of 94.66% and a molar yield of 61.42%. The resulting β-menaquinone crystal had a melting point of 105.6°C.

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Abstract

The invention discloses a method for promoting beta-menadione production through ultrasonic waves. The method includes the steps that oxidation liquid is prepared from sodium bichromate and sulfuric acid, the oxidization liquid is slowly added into mixed mediums containing beta-methyl naphthalene, phase transfer catalysts and water to undergo reaction, and the ultrasonic waves act on the reaction system in the reacting process. Due to the fact that the ultrasonic waves have the promotion effect on the reaction, the temperature of the reaction system can be greatly lowered, side reactions are reduced, the product yield is improved, and the using amount of the oxidization liquid can be greatly reduced.

Description

technical field [0001] The invention relates to a method for promoting the production of β-menadione by ultrasonic waves. Background technique [0002] 2-methyl-1,4-naphthoquinone (abbreviated as β-menadione, also known as vitamin K3, 2-MNQ, β-MNQ), is used as a synthetic anti-hemorrhagic drug in medicine. Mainly involved in the synthesis of hepatic thrombin and promoting the synthesis of plasma coagulation factors in the liver, it is indispensable to maintain the function of the blood coagulation mechanism system. β-menadione is one of the classic hemostatic agents, so β-menaquinone is also called anti-bleeding factor. Lack of β-menadione will lead to decreased coagulation factor activity and prolonged coagulation time. [0003] β-menaquinone has anti-inflammatory, cough-relieving, analgesic effects, and can treat diseases such as hepatitis, enteritis, and dysentery. It also has significant clinical effects in inhibiting tumors and anti-cancer. As a feed additive, β-mena...

Claims

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Application Information

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IPC IPC(8): C07C50/12C07C46/04
CPCC07C46/04C07C50/10
Inventor 李先荣陈宁董明甫秦龙黄玉西
Owner SICHUAN YINHE CHEM
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