The synthetic method of pentafluorobenzonitrile

A technology of pentafluorobenzonitrile and synthetic methods, which is applied in chemical instruments and methods, preparation of carboxylic acid nitriles, preparation of organic compounds, etc., and can solve problems such as high raw material prices, complicated industrialization, and no practical significance

Active Publication Date: 2021-04-16
SHANDONG HIMILE CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] (3) With pentabromobenzonitrile and potassium fluoride as raw materials, react in a pressure vessel at 300° C.; the raw material price of this method is high and has no practical significance;
[0020] Although microreactors have the above-mentioned advantages, the article also mentions that the main disadvantages of microreactors are that "industrialization is complicated: first, the number of micro-equipment increases, although the cost of amplification is reduced, but its processing capacity is still small; secondly, micro-reactors Scaling up the reactor seemed simple, but it was a huge challenge to realize it."

Method used

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  • The synthetic method of pentafluorobenzonitrile
  • The synthetic method of pentafluorobenzonitrile
  • The synthetic method of pentafluorobenzonitrile

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0065] A 316L stainless steel microreactor purchased from Shandong Haomai Chemical Technology Co., Ltd. was used, which included 10 reaction chambers. The size of the connecting channel is 1mm, the total liquid holding capacity of the microreactor is 100mL, and the outlet of the reactor is connected to gas-liquid separation.

[0066] Dilute benzonitrile with acetonitrile to 20% by weight, feed at 30mL / min through a feed pump, and feed 10 volume% fluorine at 88g / min through a pressure reducing valve, and the feed positions are all in the first reaction chamber . The reaction temperature is controlled at 10° C., and the reaction pressure is controlled at 2 MPa. After being stable for 15 minutes, switch to the quantitative collection tank to collect the product quantitatively for 60 minutes. After rectification and separation, the product content is 99.1% by sampling and analysis, and the single-pass product yield is 21.7%.

[0067] After 2 hours of reaction, it was found that ...

Embodiment 2

[0069] A 316L stainless steel microreactor purchased from Shandong Haomai Chemical Technology Co., Ltd. was used, which included 10 reaction chambers. The size of the connecting channel is 1mm, the total liquid holding capacity of the microreactor is 100mL, and the outlet of the reactor is connected to gas-liquid separation.

[0070] Dilute benzonitrile with acetonitrile to 20% by weight, feed at 30mL / min by feed pump, feed 10 volume% fluorine with 88g / min by pressure reducing valve, the feeding position of benzonitrile solution is the first One reaction chamber, and the feeding position of fluorine gas is the first and the fourth reaction chamber. The reaction temperature is controlled at 10° C., and the reaction pressure is controlled at 2 MPa. After being stable for 15 minutes, switch to the quantitative collection tank to collect the product quantitatively for 60 minutes. After rectification and separation, take a sample to analyze the product content of 98.9%, and calcul...

Embodiment 3

[0073] A 316L stainless steel microreactor purchased from Shandong Haomai Chemical Technology Co., Ltd. was used, which included 10 reaction chambers. The size of the connecting channel is 1mm, the total liquid holding capacity of the microreactor is 100mL, the outlet of the reactor is connected to a stainless steel microtube reactor with an outer diameter of 3mm, the total volume is 40mL, immersed in a cold trap, and the temperature is controlled at 10°C; the outlet of the microtube reactor is connected to gas liquid separation.

[0074] Dilute benzonitrile to 20% with acetonitrile, feed from the first reaction chamber at 30mL / min through the feed pump, and feed 10% fluorine gas from the first and fourth reaction chambers at 88g / min through the pressure reducing valve The chamber is divided into two feeds. The reaction temperature is controlled at 10° C., and the reaction pressure is controlled at 2 MPa. After being stable for 15 minutes, switch to the quantitative collecti...

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Abstract

A synthesis method of pentafluorobenzonitrile is disclosed, which includes the step of fluorinating benzonitrile with fluorine gas. The synthesis method of pentafluorobenzonitrile uses a microreactor, and the microreactor includes a plurality of series The reaction chamber, the fluorine gas is distributed and fed from the first chamber and one or more other chambers.

Description

technical field [0001] The present invention relates to a new synthetic route of pentafluorobenzonitrile. The method of the invention can advantageously synthesize pentafluorobenzonitrile continuously, safely and simply. Background technique [0002] Pentafluorobenzonitrile (CAS No.: 773-82-0) is a colorless liquid with a melting point of 2.4°C, a boiling point of 162-164°C, a molecular weight of 193, and is volatile at room temperature. [0003] Pentafluorobenzonitrile is an important fluorine-containing intermediate, which is widely used in the synthesis of pesticides, medicines, liquid crystals, catalysts and fluorine-containing materials. E.g: [0004] -In terms of medicine: due to the high content of active fluorine atoms, it can be converted into pentafluorobenzoic acid after hydrolysis, and then reduced to tetrafluorobenzoic acid after hydrogenation. Tetrafluorobenzoic acid can be used to synthesize lomefloxacin and ofloxacin , sparfloxacin, etc. as starting materi...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C07C253/30C07C255/50B01J19/00
CPCB01J19/0093C07C253/30C07C255/50
Inventor丁全有李日翔刘瑞娟杨安明苑广凤
OwnerSHANDONG HIMILE CHEM TECH