Synthetic method of camphorquinone
A synthetic method and technology of camphorquinone, applied in the field of camphorquinone synthesis, can solve problems such as high cost and complex process, achieve low production cost, simplify synthetic route, and broaden the application range
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[0038] Example 1:
[0039] Add 28g (0.2mole) α-pinene and 50ml n-hexane into a 250ml four-neck flask equipped with a thermometer, agitator, drying tube and HCl absorption device, and cool to the system temperature at -5~0℃ in an ice-salt bath . Weigh 117g (2mole) of sodium chloride into a 250ml three-necked flask, drop 53.3ml (1mole) of concentrated sulfuric acid with a constant pressure dropping funnel, and pass the generated HCl gas into α-pinene after being dried by anhydrous chlorine CaCl2 In the n-hexane solution, the reaction is about 8h, until the HCl gas is no longer absorbed. The obtained reaction solution was washed with 10% NaHCO3 solution to remove excess HCl, the organic layer was dried over anhydrous Na2SO4, and the n-hexane was evaporated under normal pressure to obtain the solid crude 2-chlorocamphane. Recrystallize with absolute ethanol (crude product: ethanol = 1:8-10g / ml) to obtain 31.7g of intermediate 2-chlorobornane, with a melting point of 129-131°C and a...
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[0042] Example 2:
[0043] 28g (0.2mole) α-pinene and 50ml n-hexanepentane were added to a 250ml four-neck flask equipped with a thermometer, agitator, drying tube and HCl absorption device, and dried HCl gas was introduced at room temperature to react for 6h. The resulting reaction solution uses 10% NaHCO 3 The solution was washed to remove excess HCl, and the organic layer was treated with anhydrous Na 2 SO 4 After drying and evaporating the n-pentane under normal pressure, a solid crude product of 2-chlorobornane is obtained. It was recrystallized with a small amount of n-hexane to obtain 20.5 g of intermediate 2-chlorobornane. Dissolve 25.2g (0.2mole) potassium n-pentoxide in 100ml DMF, heat to 135℃, and add 2-chlorobornane-DMF solution (17.3g (0.1mole) 2-chlorobornane into 50ml using a dropping funnel) DMF), react at this temperature for 4h. After the reactants are cooled, add 100ml of water and extract 3 times with 100ml of n-hexane. The extract is washed with water until ...
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