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Preparation method of fluorobenzonitrile compounds

A technology of fluorobenzonitriles and compounds, which is applied in the field of preparation of fluorobenzonitriles, to achieve the effects of speeding up the reaction, increasing sensible heat, and simplifying the product separation process

Active Publication Date: 2018-03-13
DALIAN QIKAI MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Nevertheless, there is still much room for improvement in the prior art

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  • Preparation method of fluorobenzonitrile compounds
  • Preparation method of fluorobenzonitrile compounds
  • Preparation method of fluorobenzonitrile compounds

Examples

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Effect test

Embodiment 1 5

[0079] The preparation of embodiment 1 pentafluorobenzonitrile

[0080] ① Fluorination: In a 10L fluorination autoclave equipped with a flash condenser and a receiving tank, add 1000g (3.6mol) of pentachlorobenzonitrile, 1280g (21.6mol) of anhydrous potassium fluoride and pentafluorobenzonitrile respectively. Nitrile 3000g (15.4mol), nitrogen replacement three times, remove the air in the kettle, pressurize the nitrogen to 1MPa, airtight, raise the temperature of the kettle to 280-300°C in the stirring state, keep it warm for 20h, the maximum gauge pressure of the reactor can reach 2.1MPa, Gas chromatographic analysis was performed on the still liquid sample, and the content of pentafluorobenzonitrile was 95.6%.

[0081] ②Flash: first pre-cool the flash condenser and tail gas trap on the receiving tank with the cooling medium, then slowly open the flash outlet valve of the fluorinated autoclave, and control the temperature of the condensate in the flash condenser not to exceed...

Embodiment 2 5

[0082] The preparation of embodiment 2 pentafluorobenzonitriles

[0083] ① Fluorination: In a 10L fluorination autoclave equipped with a flash condenser and a receiving tank, add 1000g (3.6mol) of pentachlorobenzonitrile, 1280g (21.6mol) of anhydrous potassium fluoride and pentafluorobenzonitrile respectively. Nitrile 5000g (25.6mol), nitrogen replacement three times, remove the air in the kettle, pressurize the nitrogen to 1MPa, airtight, raise the temperature of the kettle to 320-340°C in the stirring state, keep it warm for 20h, the maximum gauge pressure of the reactor can reach 2.8MPa, Gas chromatographic analysis was performed on the still liquid sample, and the content of pentafluorobenzonitrile was 98.7%.

[0084] ②Flash: first pre-cool the flash condenser and tail gas trap on the receiving tank with the cooling medium, then slowly open the flash outlet valve of the fluorinated autoclave, and control the temperature of the condensate in the flash condenser not to excee...

Embodiment 3

[0085] The preparation of embodiment 3 pentafluorobenzonitriles

[0086] ① Fluorination: In a 10L fluorination autoclave equipped with a flash condenser and a receiving tank, add 1000g (3.6mol) of pentachlorobenzonitrile, 1280g (21.6mol) of anhydrous potassium fluoride and pentafluorobenzonitrile respectively. Nitrile 4000g (20.5mol), nitrogen replacement three times, remove the air in the kettle, pressurize the nitrogen to 1MPa, seal it, raise the temperature of the kettle to 240-250°C in the stirring state, keep it warm for 8h, the maximum gauge pressure of the reactor can reach 1.6MPa, Gas chromatographic analysis was performed on the still liquid sample, and the content of pentafluorobenzonitrile was 95.1%.

[0087] ②Flash: first pre-cool the flash condenser and tail gas trap on the receiving tank with the cooling medium, then slowly open the flash outlet valve of the fluorinated autoclave, and control the temperature of the condensate in the flash condenser not to exceed ...

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Abstract

The present invention provides a fluorobenzonitrile compound preparation method, fluorobenzonitrile compounds are as shown in the general formula (I), an objective product can be prepared from a general-formula-(II)-shown chlorobenzonitrile compound as a raw material by reacting with an anhydrous fluoride in the presence of an inert gas under high temperature high pressure reaction conditions and flashing a reaction product, wherein the objective product itself is used as a solvent. Due to use of the objective product itself as the solvent, a main component of the fluorine exchange reaction product only comprises the objective product, due to use of an inert gas pressurization method to improve the fluorine exchange reaction and product separation conditions, the product is separated and purified in the flashing manner, the reaction residual heat is rationally used, and the whole process is simple and feasible. The method is readily available in raw materials, simple in process, energy-saving, consumption-reducing, and more suitable for industrial scale production.

Description

technical field [0001] The invention relates to a preparation method of fluorobenzonitrile compounds, belonging to the technical field of organic synthesis. Background technique [0002] Fluorobenzonitrile compounds with the general formula (I) are very important organic intermediates and are widely used in the fields of medicine, pesticides, dyes, polymer materials and liquid crystal materials. For example, 2,4,5-trifluorobenzonitrile can be used to produce oxytocin receptor antagonists, which are drugs for the treatment of premature labor. 3,4,5-Trifluorobenzonitrile can be used to synthesize 1-(3,4,5-trifluorophenyl)-2-[trans-4′-(trans-4′-n-propyl)cyclohexyl] Ethane, which is a good liquid crystal material. 2,3,5,6-tetrafluorobenzonitrile can be used to synthesize transfluthrin, which is a hygienic pyrethrin insecticide with high efficiency and low toxicity. 2,3,4,5,6-Pentafluorobenzonitrile can be used to synthesize fluoroquinolone antibacterial drugs such as sfloxaci...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C253/30C07C255/50C07C255/51
CPCC07C253/30C07C255/50C07C255/51
Inventor 侯光姜殿平
Owner DALIAN QIKAI MEDICAL TECH
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