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A technology of fluoronaphthalene and naphthylamine, which is applied in the field of preparation of the key intermediate 1-fluoronaphthalene, can solve problems such as many influencing factors, difficulty in realizing industrial production, harsh reaction conditions, etc., and achieve the goal of improving product yield and safety Effect
Active Publication Date: 2012-07-11
ZHEJIANG YONGTAI TECH CO LTD
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These two types of reaction conditions are harsh, difficult to control, high cost, poor safety, and industrial production is difficult to achieve
The third is to use fluorine to replace other halogens for fluorination. This kind of reaction is used in industry, but its application range is limited, and there are many influencing factors, it is difficult to control, and the cost is
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Embodiment 1
[0029] Embodiment 1: the preparation of diazonium fluoroborate
[0030] Put 225g of 30% HCl into a 1000ml four-necked bottle, slowly add 72g (0.5mol) of 1-naphthylamine, then cool to -10°C, add 85g of ice, 144ml of water, and then drop in sodium nitrite solution (sodium nitrite 41.4g+ Prepared with 60ml of water), the dropwise addition process ensures that the temperature is controlled at -5-0°C, after the addition is complete, stir for 30 minutes.
[0031] Slowly add 176g of 40% fluoboric acid dropwise. During the dropwise addition, the viscosity increases. After the dropwise addition, stir for 15 minutes, filter and dry, rinse with ice methanol 100ml three times, and then filter dry. The solid weighs 115g. Return the solid to a dry four-necked flask, add 150ml of toluene, stir for 30min, and filter with suction. Then beat with 100 ml of toluene, stir and filter until dry, and weigh 110 g of the obtained diazonium fluoroborate (moisture content 0.1%, toluene content 1.0%). ...
Embodiment 2
[0032] Embodiment 2: the preparation of diazonium fluoroborate
[0033] According to Example 1, the amount of 40% fluoboric acid is reduced to 143g, the solid viscosity is too large, and it is difficult to stir. After suction filtration to dryness, the obtained diazofluoroborate weighs 95g (moisture content 0.25%, Toluene content 1.5%).
Embodiment 3
[0034] Embodiment 3: the preparation of diazonium fluoroborate
[0035] According to Example 1, sulfuric acid was used instead of hydrochloric acid, and the obtained diazonium fluoroborate weighed 102 g (moisture content 0.2%, toluene content 1.2%).
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Abstract
The invention provides a method for preparing 1-fluoronaphthalene. The method comprises the following steps of: (1) reacting 1-naphthylamine serving as a raw material and a diazo reagent under acidic conditions to obtain diazonium salt; (2) reacting the diazonium salt obtained in step (1) and fluoroboric acid, phosphorofluoridic acid or salt of the fluoroboric acid and the phosphorofluoridic acid to obtain crude diazonium fluoroborate or crude diazonium fluorophosphate; and (3) replacing and dehydrating the diazonium fluoroborate or the crude diazonium fluorophosphates by using alcohol, replacing the alcohol by using a solvent formed by one or more of methylbenzene, benzene, dimethylbenzene, chlorobenzene, nitrobenzene, chloroform, dichloromethane, dichloroethane, trichloroethylene, cyclohexane and n-hexane, and directly cracking to obtain the 1-fluoronaphthalene. By the method, the technical problem that the diazonium salt is easy to decompose when dried and dehydrated in the traditional process is solved, and the yield and safety of the product are improved; the process is simple, and the industrialization is easy to realize; and the product has high purity and stable characteristics, and fully meets the using requirements when taken as a pharmaceutical intermediate.
Description
technical field [0001] The present invention relates to the technical field of preparation methods of pharmaceutical intermediates, and further relates to the field of preparation methods of 1-fluoronaphthalene, a key intermediate of the antidepressant drug duloxetine. Background technique [0002] In industrialized countries, depression is the most common mental illness, and the lifetime incidence of depression is between 6% and 8%. There are 15 million adults in the United States suffering from depression. With the gradual aging of the population and society, the incidence of depression among people over 60 years old will be as high as 20%-50%. It is predicted that by 2010, the incidence of depression in these countries will increase to about 8%-10%. According to the "2002 World Health Report" published by the World Health Organization, depression has become the fourth largest disease in the world, and by 2020, depression may become the second largest disease after heart ...
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