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Synthesis method of 2-ethyl-1-fluoro-4-nitrobenzene

A synthesis method and technology of nitrobenzene, which are applied in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc., can solve problems such as no problems, and achieve the effects of easy operation, high yield, and easy popularization and use.

Pending Publication Date: 2022-05-17
江苏壹药新材料有限公司
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] 2-Ethyl-1-fluoro-4-nitrobenzene is a derivative of nitrobenzene, which plays an important role and has wide application value, but there is no report on its synthesis, and the current market is also Need a kind of synthetic method of 2-ethyl-1-fluoro-4-nitrobenzene badly, carry out use

Method used

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  • Synthesis method of 2-ethyl-1-fluoro-4-nitrobenzene

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[0015] A kind of synthetic method of 2-ethyl-1-fluoro-4-nitrobenzene, this synthetic method comprises the steps:

[0016] (1) Take the material according to the mass ratio of compound A, concentrated sulfuric acid, and nitric acid solution with a mass fraction of 65% of 1:7 to 10:1, add concentrated sulfuric acid to the reactor, cool to 0°C, and add compound A , stir, then add a nitric acid solution with a mass fraction of 65%, keep warm, rise to 30-35°C, stir, compound B;

[0017] (2) According to compound B, the mass ratio of sodium nitrite is 2:1, the mass fraction is 50% fluoboric acid solution, and the volume ratio of p-xylene is 1:1, the mass fraction is 50% fluoboric acid solution and sodium nitrite The liquid-solid mL / g ratio is 40:1, take the material, put compound B and 50% fluoroboric acid solution into the reactor, cool down to 0°C, add sodium nitrite, stir the reaction, filter, collect For the filter cake, add p-xylene into the reactor, heat to 120-130°C, add the...

Embodiment 1

[0019] A kind of synthetic method of 2-ethyl-1-fluoro-4-nitrobenzene, this synthetic method comprises the steps:

[0020] (1) Add 140g of concentrated sulfuric acid to the reactor, cool to 0°C, add 20g of compound A, stir for 20min, then add 80g of nitric acid solution with a mass fraction of 65%, keep it warm for 1h, rise to 30°C, stir for 15h, and obtain TLC Detection, the reaction of the raw materials is completed, the reaction solution is poured into ice water, the pH is adjusted to 8-9 with 20% aqueous sodium hydroxide solution, 800 mL of ethyl acetate is added, filtered with diatomaceous earth, the liquid is separated, and the aqueous phase is extracted with ethyl acetate (400 mL ), combined the organic phase, mixed the sample with silica gel and passed the column, mobile phase: n-hexane / ethyl acetate=5 / 1, collected the target product, concentrated to obtain 26.3g yellow solid, and obtained compound B with a yield of 95.9% and a purity of 98.3 %;

[0021] (2) Put 20g of...

Embodiment 2

[0024] A kind of synthetic method of 2-ethyl-1-fluoro-4-nitrobenzene, this synthetic method comprises the steps:

[0025] (1) Add 160g of concentrated sulfuric acid to the reactor, cool to 0°C, add 20g of compound A, stir for 20min, then add 80g of nitric acid solution with a mass fraction of 65%, keep it warm for 1h, rise to 33°C, stir for 15h, and obtain TLC Detection, the reaction of the raw materials is completed, the reaction solution is poured into ice water, the pH is adjusted to 8-9 with 20% aqueous sodium hydroxide solution, 800 mL of ethyl acetate is added, filtered with diatomaceous earth, the liquid is separated, and the aqueous phase is extracted with ethyl acetate (400 mL ), combined the organic phase, mixed the sample with silica gel and passed the column, mobile phase: n-hexane / ethyl acetate=5 / 1, collected the target product, concentrated to obtain 26.5 yellow solids, and obtained compound B with a yield of 96.6%;

[0026] (2) Put 20g of compound B and 400mL of...

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Abstract

The invention belongs to the technical field of chemical intermediate synthesis, and particularly relates to a synthetic method of 2-ethyl-1-fluoro-4-nitrobenzene. The 2-ethyl-1-fluoro-4-nitrobenzene is prepared from the compound A as a raw material through nitration and Balz-Schiemann reaction, the synthesis method is simple and easy to operate, and the obtained product is high in yield, high in purity and easy to popularize and use.

Description

technical field [0001] The invention belongs to the technical field of chemical intermediate synthesis, and in particular relates to a synthesis method of 2-ethyl-1-fluoro-4-nitrobenzene. Background technique [0002] Nitrobenzene, is an organic compound with the chemical formula C 6 h 5 NO 2 , a colorless or yellowish oily liquid with a bitter almond flavor. Hardly soluble in water, denser than water, easily soluble in ethanol, ether, benzene and oil. It will burn and explode in case of open flame or high heat. Reacts violently with nitric acid. Often used as organic synthesis intermediates and raw materials for the production of aniline, used in the production of dyes, spices, explosives and other organic synthesis industries. [0003] 2-Ethyl-1-fluoro-4-nitrobenzene is a derivative of nitrobenzene, which plays an important role and has wide application value, but there is no report on its synthesis, and the current market is also There is an urgent need for a synth...

Claims

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Application Information

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IPC IPC(8): C07C201/12C07C205/12C07C209/76C07C211/52
CPCC07C201/12C07C209/76C07C211/52C07C205/12
Inventor 李小明刘芝英
Owner 江苏壹药新材料有限公司
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