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CoenzymeQ 0quinhydrones normal pressure catalytic hydrogenation preparation process and its refining method

A technology of catalytic hydrogenation and preparation process, which is applied in the direction of chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as recrystallization, large product loss, and difficult operation, so as to improve yield and purity, avoid Product loss, cost reduction effects

Inactive Publication Date: 2006-04-26
YUNNAN KEEN BIOENG
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  • Claims
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Problems solved by technology

For the hydrogen reduction system, it is generally carried out under relatively high pressure, requiring high-pressure equipment, difficult to operate, and the usual recrystallization of sulfur dioxide aqueous solution, the product loss is relatively large, and the product is not easy to dry, which is not conducive to large-scale industrial production

Method used

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  • CoenzymeQ 0quinhydrones normal pressure catalytic hydrogenation preparation process and its refining method
  • CoenzymeQ 0quinhydrones normal pressure catalytic hydrogenation preparation process and its refining method

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Embodiment

[0012] figure 1 In, 2,3-dimethoxy-5-methyl-1,4-benzoquinone (coenzyme Q 0 ) 18.2g was dissolved in 60ml of absolute ethanol, 1g of palladium carbon catalyst was added, and hydrogenation reaction was carried out under normal pressure. Remove the solvent, obtain 17.5g coenzyme Q 0 Hydroquinone, yield 95%. The melting point is 77-78°C.

[0013] 5 g of 2,3-dimethoxy-5-methyl-1,4-benzoquinone was dissolved in 200 mL of methanol, and hydrogenated with a palladium black (5% palladium) catalyst at a pressure of 50 psi. After the hydrogen absorption stopped, the catalyst was filtered off, and the filtrate was concentrated under reduced pressure. The residue was dissolved in 35 mL of water containing some sulfur dioxide, and the solution was cooled overnight. Collect the precipitated crystals to obtain coenzyme Q 0 Hydroquinone 2.88g, melting point 77~78℃. After the filtrate was concentrated, 0.78 g of the product was also recovered, with a total yield of 73%.

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Abstract

The present invention relates to the normal pressure catalytic hydrogenation process of preparing coenzyme Q0 hydroquinone and the refining process. The preparation and refining process includes mainly the normal pressure catalytic hydrogenation of coenzyme Q0 under the action of 5 % Pd / C catalyst, and washing with non-polar solvent for refining to eliminate un-reacted matter and impurity. The process has no high pressure operation, easy separation of product and no water related operation to result in loss of the product, so that the present invention has high product yield and purity and low cost.

Description

technical field [0001] The present invention relates to a kind of coenzyme Q 0 Atmospheric pressure catalytic hydrogenation preparation process of hydroquinone and its refining method. Background technique [0002] coenzyme Q 0 hydroquinone is the production of coenzyme Q n , vitamin K and important intermediates of many natural quinones. There are many ways to reduce quinones, including H 2 / Pt,H 2 / Pd [JP-A-38-26372, JP-A-39-17513, JP-A-39-17514], LiAlH 4 , NaBH 4 , LiAlH(OR) 3 , SnCl 2 , Sn / HCl, , Zn / CH 3 COOH, Zn / NH 4 OH, TiCl 3 , VCl 2 , CrCl 2 , C 6 h 5 NHNH 2 , H 2 S, SO 2 , Na 2 S 2 o 4 [Agric.Biol.Chem., 49(10), 3071,1985; M.Hudlicky.Reduction in Organic Chemistry.Ellis Horwood Itd., 1984] for the reduction of water system, due to coenzyme Q 0 Hydroquinone has a certain solubility, and product separation is difficult. For the hydrogen reduction system, it is generally carried out under relatively high pressure, which requires high-pressure e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/253C07C41/26
Inventor 张建臣
Owner YUNNAN KEEN BIOENG
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