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Synthesis method of 1-fluoronaphthalene

A synthetic method and technology of fluoronaphthalene, applied in the field of synthesis of 1-fluoronaphthalene, capable of solving the problems of low yield of 1-fluoronaphthalene

Pending Publication Date: 2022-01-28
武汉瑞阳化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The object of the present invention is to overcome above-mentioned technical deficiency, provide a kind of synthetic method of 1-fluoronaphthalene, solve the low technical problem of the yield of 1-fluoronaphthalene in the prior art

Method used

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  • Synthesis method of 1-fluoronaphthalene

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[0019] This specific embodiment provides a kind of synthetic method of 1-fluoronaphthalene, comprises the following steps:

[0020] S1, adding menaphthylamine to anhydrous hydrofluoric acid below 10°C to form menaphthylamine hydrofluoride; the mass ratio of said anhydrous hydrofluoric acid to said menaphthylamine is (2-5):1 ;

[0021] S2. Add anhydrous nitrite to the menaphthylamine hydrofluoride, and perform a diazotization reaction below 5°C to obtain an α-diazonaphthyl hydrofluoride solution; the anhydrous nitrate and the The mass ratio of menaphthylamine hydrofluoride is 1:(1.8-2); Further, described anhydrous nitrite is anhydrous sodium nitrite or anhydrous potassium nitrite;

[0022] S3. Thermally decomposing the α-diazonaphthalene hydrofluoride solution in a thermal decomposer at 50-80° C. to obtain a solution containing 1-fluoronaphthalene;

[0023] S4. Layering the solution containing 1-fluoronaphthalene to obtain a lower organic layer and an upper acid layer, neutr...

Embodiment 1

[0028] The present embodiment proposes a kind of synthetic method of 1-fluoronaphthalene, comprises the following steps:

[0029] S1, adding menaphthylamine to anhydrous hydrofluoric acid at 5°C to form menaphthylamine hydrofluoride; the mass ratio of said anhydrous hydrofluoric acid to said menaphthylamine is 3:1; menaphthylamine It is a block solid below 50°C, so menaphthylamine needs to be crushed into powder and then fed with an auger;

[0030] S2. Add anhydrous sodium nitrite to the menaphthylamine hydrofluoride, and perform a diazotization reaction at 5° C. to obtain an α-diazonaphthyl hydrofluoride solution; the anhydrous nitrate and the The mass ratio of menaphthylamine hydrofluoride is 1:1.8; Anhydrous nitrite is solid, therefore adopts auger to continuously and slowly wring in menaphthylamine hydrofluoride;

[0031] S3. Thermally decompose the α-diazonaphthalene hydrofluoride solution in a thermal decomposer at 50° C. to obtain a solution containing 1-fluoronaphthal...

Embodiment 2

[0034] The present embodiment proposes a kind of synthetic method of 1-fluoronaphthalene, comprises the following steps:

[0035] S1, adding menaphthylamine to anhydrous hydrofluoric acid at 8°C to form menaphthylamine hydrofluoride; the mass ratio of said anhydrous hydrofluoric acid to said menaphthylamine is 2:1; menaphthylamine It is a block solid below 50°C, so menaphthylamine needs to be crushed into powder and then fed with an auger;

[0036] S2. Add anhydrous sodium nitrite to the menaphthylamine hydrofluoride, and perform a diazotization reaction below 3°C to obtain an α-diazonaphthyl hydrofluoride solution; the anhydrous nitrate and the The mass ratio of menaphthylamine hydrofluoride is 1:2; Anhydrous nitrite is solid, so adopts auger to continuously slowly wring in menaphthylamine hydrofluoride;

[0037] S3. Thermally decompose the α-diazonaphthalene hydrofluoride solution in a thermal decomposer at 60°C to obtain a solution containing 1-fluoronaphthalene; at this t...

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Abstract

The invention discloses a synthesis method of 1-fluoronaphthalene, and belongs to the technical field of synthesis of 1-fluoronaphthalene. The synthesis method of 1-fluoronaphthalene comprises the following steps: S1, adding menaphthylamine into anhydrous hydrofluoric acid to form menaphthylamine hydrofluoride; S2, adding anhydrous nitrite into the methylnaphthylamine hydrofluoride, and carrying out diazotization reaction to obtain an alpha-diazo naphthalene hydrofluoride solution; and S3, carrying out thermal decomposition on the alpha-diazonaphthalene hydrofluoride solution at 50-80 DEG C to obtain a solution containing 1-fluoronaphthalene. The yield of the 1-fluoronaphthalene obtained by the synthesis method provided by the invention is more than 80%.

Description

technical field [0001] The invention relates to the technical field of synthesis of 1-fluoronaphthalene, in particular to a synthesis method of 1-fluoronaphthalene. Background technique [0002] At present, the production of 1-fluoronaphthalene is generally used in the hydrochloric acid medium, menaphthylamine and hydrochloric acid to generate hydrochloride, and then diazotized by adding sodium nitrite aqueous solution dropwise at low temperature, and then dropwise added fluoroboric acid to form diazonium Fluoroborate, then centrifuged, dried and thermally decomposed to obtain crude 1-fluoronaphthalene, and finally purified to obtain the product. In this process, it is difficult to dry the diazonium salt, which leads to the easy generation of by-products in the thermal decomposition process, and finally makes the yield of 1-fluoronaphthalene low. Contents of the invention [0003] The purpose of the present invention is to overcome above-mentioned technical deficiency, pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/093C07C25/22
CPCC07C17/093C07C245/20C07C25/22
Inventor 万洪周琴万科辰
Owner 武汉瑞阳化工有限公司
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