Preparation method for 3,5-dibenzoyl-2-deoxy-2-fluoro-2-methyl-D-ribono-gamma-lactone

A technology of dibenzoyl and methyl groups, applied in the field of medicine, can solve the problems of difficulty in purifying starting materials, corrosion of enamel kettle equipment, and incompatibility with large-scale production, and achieves alleviation of environmental pressure in factories, low prices, and three wastes small amount of effect

Active Publication Date: 2016-11-09
杭州惠诺医药科技有限公司
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Problems solved by technology

The starting material used in this method is difficult to purify, so it is not easy to purchase. Thionyl chloride is used to undergo thionylation, and sodium hypochlorite oxidative sulfonylation will cause a large amount of waste water in the reaction. Fluorination with triethylamine t

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  • Preparation method for 3,5-dibenzoyl-2-deoxy-2-fluoro-2-methyl-D-ribono-gamma-lactone
  • Preparation method for 3,5-dibenzoyl-2-deoxy-2-fluoro-2-methyl-D-ribono-gamma-lactone
  • Preparation method for 3,5-dibenzoyl-2-deoxy-2-fluoro-2-methyl-D-ribono-gamma-lactone

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[0046] The present invention will be described below with specific examples. It should be understood that examples are used to illustrate the present invention rather than to limit the present invention, and the scope and core content of the present invention are determined according to the claims.

[0047] A preparation method of 3,5-dibenzoyl-2-deoxy-2-fluoro-2-methyl-D-ribose-γ-lactone of the present invention specifically comprises the following steps:

[0048] 1) First add 500L of acetone to the reaction kettle, then add 100kg of D-mannitol and 1kg of stannous chloride in batches, and stir for 1 hour. Add 120kg of 2,2-dimethoxypropane under temperature control at 20°C-25°C, raise the temperature to 35-40°C and react for 5 hours. After the reaction was completed, the acetone was removed by concentration under reduced pressure, and the residue was added with dichloromethane and stirred evenly. About 500 L of saturated aqueous sodium carbonate solution was added to another ...

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Abstract

The invention discloses a preparation method for 3,5-dibenzoyl-2-deoxy-2-fluoro-2-methyl-D-ribono-gamma-lactone. The preparation method comprises the following steps: subjecting a starting raw material D-mannitol to acetone protection and sodium periodate oxidation; then subjecting the treated D-mannitol and a self-made ylide reagent to the Witting reaction; then carrying out selective oxidation by using an aqueous sodium permanganate solution; then successively carrying out sulfonylation, fluorination with potassium fluoride, and ring closing with a concentrated protective group protective group; protecting the hydroxyl group by using benzoyl chloride; and then carrying out purification so as to obtain the final product 3,5-dibenzoyl-2-deoxy-2-fluoro-2-methyl-D-ribono-gamma-lactone. The preparation method provided by the invention uses easily available and cheap raw materials, so production cost is greatly reduced; and the operation of the preparation method is coherent and simple, and the quantity of waste gas, waste water and industrial residues is lower than the quantity of waste gas, waste water and industrial residues reported in the prior art.

Description

technical field [0001] The invention belongs to the field of medicine, and in particular relates to a preparation method of 3,5-dibenzoyl-2-deoxy-2-fluoro-2-methyl-D-ribose-γ-lactone. Background technique [0002] Viral hepatitis type C (hepatitis C for short), is a disease caused by hepatitis C virus (HCV) infection, and is mainly transmitted through blood. Clinical manifestations include fever, gastrointestinal symptoms, and abnormal liver function. Similar to hepatitis B, but milder. Most cases are subclinical, with severe chronicity, which can also lead to fulminant hepatic failure. More common in co-infection with other viruses. [0003] According to UN news reports, three to four million people are infected with hepatitis C virus every year. About 150 million people suffer from chronic hepatitis C and are at risk of developing liver cirrhosis or liver cancer, and more than 350,000 people die from hepatitis C-related liver diseases every year. China is also a large...

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Application Information

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IPC IPC(8): C07D307/33
CPCY02P20/55C07D307/33
Inventor 韩方津
Owner 杭州惠诺医药科技有限公司
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