Method for preparing vitamin K3

A vitamin and methyl technology, applied in the field of vitamin K3 preparation, can solve the problems of poor reaction selectivity, complicated post-treatment, high reaction temperature, etc., and achieve the effects of mild reaction conditions, stable process, and simplified operation steps

Inactive Publication Date: 2015-11-11
COMPREHENSIVE TECH SERVICE CENT OF QUANZHOU ENTRY EXIT INSPECTION & QUARANTINE BUREAU OF P R C
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Problems solved by technology

2-Methyl-1,4-naphthoquinone is the earliest vitamin K3 used by people. It has high activity and low price, but it has poor stability and is not easy to absorb. Then people developed a new type of easily absorbed vitamin K3 (sodium bisulfite men

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  • Method for preparing vitamin K3

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Experimental program
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Effect test

Embodiment 12

[0030] The preparation of embodiment 12-methyl-1,4-naphthoquinone

[0031] At 15°C, after dissolving 2-methylnaphthalene (1kg) in n-hexane (2L), add sodium dodecylsulfonate (0.1Kg) and 2.75mol / L chromium ion oxidation solution (35L), Stir mechanically, after reacting for 3 hours, put the reaction solution in the refrigerator to freeze (-18°C) for crystallization for 6 hours, filter with suction, wash with water to obtain a filter cake, which is confirmed to be 2-methyl-1,4-naphthalene by NMR detection The quinone was weighed after drying, the yield was 84.5%, and the purity was 97% when detected by high performance liquid chromatography.

Embodiment 1

[0032] The proton nuclear magnetic resonance spectra of the 2-methyl-1,4-naphthoquinone prepared in Example 1 can be found in figure 1 , the carbon nuclear magnetic resonance spectrogram of the 2-methyl-1,4-naphthoquinone that embodiment 1 prepares sees figure 2 .

Embodiment 22

[0033] The preparation of embodiment 22-methyl-1,4-naphthoquinone

[0034] At 45°C, after dissolving 2-methylnaphthalene (1kg) in n-hexane (2L), add sodium dodecylsulfonate (0.1kg) and 2.75mol / L chromium ion oxidation solution (14L), Stir mechanically, react for 3 hours, put the reaction solution into the refrigerator to freeze (-18°C) for crystallization for 6 hours, filter with suction, wash with water to obtain a filter cake, which is confirmed to be 2-methyl-1,4-naphthalene by nuclear magnetic resonance The quinone was weighed after drying, the yield was 89.1%, and the purity was 98.5% by high-performance liquid chromatography.

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Abstract

The invention provides a method for preparing vitamin K3, and relates to vitamin K3. The method for preparing vitamin K3 with the chemical name of 2-methyl-1,4-naphthoquinone includes the following steps: dissolving 2-methylnaphthalene into a hydrocarbon solvent; adding sodium dodecyl sulfate and chromium ion oxidation liquid for an oxidation reaction; after completion of the reaction, purifying the reaction solution to obtain vitamin K3 with the chemical name of 2-methyl-1,4-naphthoquinone. The method for preparing vitamin K3 with the chemical name of 2-methyl-1,4-naphthoquinone sodium bisulfate includes the following steps: dissolving 2-methyl-1,4-naphthoquinone into a mixed solvent of water and ethyl alcohol; then adding sodium bisulfite for a sulfonation reaction; after completion of the reaction, purifying the reaction solution to obtain vitamin K3 with the chemical name of 2-methyl-1,4-naphthoquinone sodium bisulfate. According to the invention, the method is high in reaction selectivity, mild in reaction conditions, short in operation steps, green and environment-friendly, and stable in process; the product purity is 97% or above, and the total yield is 79% or above.

Description

technical field [0001] The invention relates to vitamin K3, in particular to a preparation method of vitamin K3. Background technique [0002] Vitamin K3 is not only an important vitamin variety, but also an important intermediate for the synthesis of K-series vitamins, such as vitamin K1 (β-methyl-3-phytyl-l,4-naphthone), vitamin K2 (β- Methyl-3-difarnesyl-1,4-naphthoquinone), etc. 2-Methyl-1,4-naphthoquinone is the earliest vitamin K3 used by people. It has high activity and low price, but it has poor stability and is not easy to absorb. Then people developed a new type of easily absorbed vitamin K3 (sodium bisulfite menadione ). The function of vitamin K3 is to promote coagulation, and the level of prothrombin in the blood is directly related to the supply of vitamin K3. Animals deficient in vitamin K3 will significantly prolong the coagulation time, and in severe deficiencies, slight abrasions will cause bleeding and lead to death. In order to promote animal growth a...

Claims

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Application Information

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IPC IPC(8): C07C50/10C07C46/04C07C46/10
CPCC07C46/04C07C46/10
Inventor 翁城武黄伙水韦航荣杰锋李亦军许彩霞连小彬吴俐
Owner COMPREHENSIVE TECH SERVICE CENT OF QUANZHOU ENTRY EXIT INSPECTION & QUARANTINE BUREAU OF P R C
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