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Preparation method for high-purity 4-fluorobenzoylacetonitrile

A -fluorobenzoylacetonitrile, high-purity technology, applied in the field of preparation of high-purity 4-fluorobenzoylacetonitrile, can solve the problems of low yield, difficult purification, large impurities, etc., and achieves a simple purification method and easy industrialization Effect

Active Publication Date: 2016-01-27
天津市科莱博瑞科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, sodium amide is used as a base, and acetonitrile and methyl p-fluorobenzoate are used to react at room temperature to prepare 4-fluorobenzoyl acetonitrile. This method will generate a large amount of impurities, which not only has a low yield, but is also difficult to purify.

Method used

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  • Preparation method for high-purity 4-fluorobenzoylacetonitrile
  • Preparation method for high-purity 4-fluorobenzoylacetonitrile
  • Preparation method for high-purity 4-fluorobenzoylacetonitrile

Examples

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Effect test

Embodiment 1

[0024] Add anhydrous tetrahydrofuran (100mL) to a 500mL three-necked flask, add sodium (3.14g), under nitrogen protection, cool to -30°C, add acetonitrile (25mL) dropwise, the temperature does not exceed 0°C, the dropwise addition is completed, At -30-0°C, the sodium reaction is complete, add dropwise a solution of 4-fluorobenzoic acid methyl ester (20g) in tetrahydrofuran (50mL), the temperature is between -30-0°C, the dropwise addition is complete, and the reaction is in this temperature range Continue the reaction in middle temperature, TLC plate monitoring, the raw material reaction is complete, dropwise add methanol (20mL) to quench the reaction, the temperature does not exceed 0 °C, the quenching is complete, adjust the pH value to 7 with 1N hydrochloric acid, separate the liquid, and use ethyl acetate for the aqueous phase Extraction, the organic phase was washed with saturated salt, dried with anhydrous sodium sulfate, concentrated to dryness under reduced pressure, and...

Embodiment 2

[0025] Add acetonitrile (100mL) into a 250mL three-neck flask, lower the temperature to -30°C, and add sodium (3.28g) in batches under nitrogen protection, the temperature does not exceed 0°C, the sodium reaction is complete, drop 4-fluorine Methyl benzoate (20g) in acetonitrile (50mL) solution, the temperature is between -30 ~ 0 ℃, the dropwise addition is completed, the reaction continues to react in this temperature range, TLC board monitoring, the raw material reaction is complete, dropwise add methanol (20mL ) to quench the reaction, the temperature does not exceed 0°C, the quenching is complete, the pH value is adjusted to 7 with 1N hydrochloric acid, the liquid is separated, the aqueous phase is extracted with ethyl acetate, the organic phase is washed with saturated salt, and dried with anhydrous sodium sulfate. Concentrate to dryness under reduced pressure, and beat with petroleum ether to obtain 20.1 g of white solid, HPLC: 99.3%, excluding 4‐methoxybenzoyl acetonitri...

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Abstract

The invention belongs to the pharmaceutical chemistry synthesis technology field, and concretely provides a preparation method for high-purity 4-fluorobenzoylacetonitrile. In the preparation method, alkali metal is employed as a base, acetonitrile is employed as a solvent, acetonitrile and methyl 4-fluorobenzoate are reacted to synthesize 4-fluorobenzoylacetonitrile. The solvent also can be a mixed liquid of acetonitrile and absolute ether. The preparation method can avoid generation of impurities 4-methoxy-benzoylacetonitrile and benzoylacetonitrile with properties extremely similar to the product, the purification mode is simple, the yield can reach more than 93%, and the product purity can reach more than 99%. The method is easy for industrialization, and the high-purity product can be obtained with high yield, thus, the preparation method has strong practicality, and the preparation method is suitable for popularization and application in correlative technology fields.

Description

technical field [0001] The invention belongs to the technical field of pharmaceutical chemical synthesis, in particular to a preparation method of high-purity 4-fluorobenzoyl acetonitrile. Background technique [0002] 4-fluorobenzoyl acetonitrile, molecular formula: C9H6FNO, structural formula is as follows: [0003] [0004] 4-Fluorobenzoyl acetonitrile is used as an intermediate of various drugs such as blonanserin for the treatment of schizophrenia, heterocyclic pyridine compounds for the prevention and treatment of cardiovascular and cerebrovascular diseases, senile dementia, hyperlipidemia, etc. The preparation method has also become one of the focuses of human attention. [0005] [0006] Patents WO2003076405, CN102030707 and other relevant documents disclose a synthesis method (Scheme 1) of 4-fluorobenzoylacetonitrile, and this method is the most concerned synthesis method. However, the product synthesized by this method will contain about 0.5% 4-methoxybenzo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/40C07C253/30
Inventor 罗建中
Owner 天津市科莱博瑞科技有限公司
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