Method for producing nicergoline

A nicergoline, production method technology, applied in chemical instruments and methods, products, chemical/physics/physicochemical processes and other directions, can solve problems such as environmental pollution, synthetic reaction quality factors, etc., achieves simple operation, sealing The effect of good performance and environmental protection, mild reaction conditions

Inactive Publication Date: 2011-09-14
HONGYI SCI & TECH CO LTD NANCHANG
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] Compared with the above two schemes, the third scheme has relatively conventional reaction conditions, but there are many factors affecting the quality of the synthesis reaction. It is difficult for the current production equipment to avoid environmental pollution during the synthesis reaction.

Method used

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  • Method for producing nicergoline
  • Method for producing nicergoline
  • Method for producing nicergoline

Examples

Experimental program
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Embodiment Construction

[0029] 1, Preparation of 10α-methoxy phoergool (II)

[0030] Under the protection of nitrogen, add 3.9LCH to the multifunctional reaction kettle with special bottom valve 3 OH / H 2 SO 4 (40 / 7.5) and ergot alcohol 130g, heated to dissolve (temperature control 35 ~ 40 ℃); ultraviolet irradiation reaction (Philips UV lamp of HPLR-N 250W, 330nm, 20 ~ 40 ℃), after the reaction, the reaction The solution was poured into about 15L of ice water, slowly added 1.7L of ammonia water, extracted with dichloromethane (4L×3), the organic layer was washed with water, and anhydrous Na 2 SO 4 After drying, the solvent was evaporated under reduced pressure, the residue was recrystallized with acetonitrile, and filtered with a special filter to obtain 102 g of product (II), with a yield of 70%.

[0031] Product quality control: Product (II) is a brown powder with a melting point of 183-187°C.

[0032] Reaction process monitoring: TLC method, silica gel GF254 plate, developer CH 3 OH: CHCl 3...

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Abstract

The invention discloses a method for producing nicergoline, which takes a multifunctional reaction kettle with a special kettle bottom valve as a reactor, a special filter as refining equipment and lysergol as an original raw material and comprises the following steps: directly carrying out photoreaction at room temperature in sulfuric acid-methanol to obtain 10alpha-methoxy optical lysergol; reacting the 10alpha-methoxy optical lysergol with methyl iodide under an alkaline condition to obtain 1-methyl-10alpha-methoxy optical lysergol; and directly forming ester with 5-bromine niacin to produce the nicergoline. Compared with the method for producing the nicergoline through current synthesis equipment, the disclosed production process of the nicergoline has the advantages of few reaction steps, mild reaction conditions, convenient refinement, simple operation, good effects of heat preservation, oxidation resistance, sealing property and environmental protection of the used special equipment, complete reaction, simple structure of reaction equipment, convenient operation, easy disassembling, assembling and cleaning, high filtering efficiency, high reaction quality and yield, and stable product quality.

Description

technical field [0001] The present invention relates to the field of medicine and chemical industry, more specifically, relate to a kind of nicergoline crude drug production method. Background technique [0002] Vascular dementia (VD) has been on the rise rapidly in recent years. With the aggravation of urbanization and aging, China's elderly population has exceeded 120 million, and the incidence of geriatric diseases is also increasing year by year. With the increase of residents' income, the requirements for the quality of life of the elderly have also increased. Under this trend, the demand for therapeutic drugs for diseases such as vascular dementia has also increased significantly. VD disease is a disease with declining function and needs long-term medication. With the development of society and the improvement of people's attention to this kind of disease, the demand for therapeutic drugs is constantly increasing. According to the results of the survey of doctors, 8....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D457/02B01J19/00
CPCY02P20/141
Inventor 刘孝乐穆正义廖新华朱丹
Owner HONGYI SCI & TECH CO LTD NANCHANG
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