Prepn process of 1-fluoronaphthalene
A technology of fluoronaphthalene and naphthylamine is applied in the field of preparation of 1-fluoronaphthalene, and can solve the problems of difficult realization of fluorinating agent equipment, difficult industrial production, and many by-products at reaction temperature.
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[0017] The preparation method of 1-fluoronaphthalene of the present invention uses 1-naphthylamine as a raw material, undergoes diazotization to form diazofluoroborate or diazofluorophosphate, and then thermally decomposes to form 1-fluoronaphthalene product.
[0018] Specifically, the preparation method of 1-fluoronaphthalene includes the following steps:
[0019] (1) Reacting 1-naphthylamine with nitrous acid, nitrite ester or nitrite in acid medium to obtain diazonium salt;
[0020] (2) reacting the diazonium salt obtained in step (1) with fluoroboric acid or its salt or fluorophosphoric acid or its salt to obtain diazonium fluoroborate or diazonium fluorophosphate;
[0021] (3) Heating and decomposing the diazofluoroborate or diazofluorophosphate obtained in step (2) to obtain 1-fluoronaphthalene.
[0022] In step (1), the acidic medium can be any medium suitable for providing an acidic environment for the diazotization reaction, including but not limited to: HCl, H 2 SO 4 Or ...
Embodiment 1
[0035] Add 143 grams (equivalent to 1 mole) of 1-naphthylamine and 400ml hydrochloric acid solution into a 2000ml four-necked flask, keep the temperature at 50~60℃ and stir for about half an hour, then cool the temperature of the reaction solution to -3℃ and add dropwise 250ml of 40% sodium nitrite aqueous solution (equivalent to 1.1 moles of sodium nitrite), the dripping is completed for about 2 hours, and the temperature is kept for about half an hour. Then, 308ml of 40% fluoroboric acid aqueous solution (equivalent to 1.4 moles of fluoroboric acid) was added dropwise, and a fine solid was formed immediately. The dropping lasted for about half an hour. After stirring for 1 hour, suction filtration, washing, and drying to obtain diazofluoroboron The acid salt solid is 222.8 grams.
[0036] Heat a 1000ml four-neck flask and control the temperature to 70~75℃. Put the diazofluoroborate solid obtained as above in batches to make it thermally decompose. After the decomposition is comp...
Embodiment 2
[0038] Add 143 grams (equivalent to 1 mole) of 1-naphthylamine and 450ml sulfuric acid solution into a 2000ml four-necked flask, keep the temperature at 60~70℃ and stir for about half an hour, then cool the temperature of the reaction solution to 5℃, and add 40% dropwise. % Sodium nitrite aqueous solution 680ml (equivalent to 3.0 moles of sodium nitrite), the dripping is completed for about 2 hours, and the temperature is kept for about half an hour. Then, 270ml of 40% sodium fluoroborate aqueous solution (equivalent to 1.2 moles of sodium fluoroborate) was added dropwise to produce a fine solid immediately. The addition lasted for about half an hour. After stirring for 1 hour, suction filtration, washing, and drying to obtain diazonium 232 grams of fluoroborate solids.
[0039]Heat a 1000ml four-neck flask and control the temperature to 140-150°C. Put the diazofluoroborate solid obtained as above in batches to make it thermally decompose. After the decomposition is completed, the...
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