Preparation method of 4-alkylresorcinol
A technology of alkylresorcinol and acylresorcinol, which is applied in the field of preparation of 4-alkylresorcinol, can solve the problems of high environmental pressure, high operation requirements, and many by-products, and reduce production Cost, ease of post-processing, effect of reducing by-products
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Embodiment 1
[0022] Add 165.0g resorcinol (1.5mol) in the 2.0L four-necked flask, then add 1.0L cyclohexane, then add 132.2g n-butyric acid (1.5mol), add 245.3g zinc chloride (1.8mol) under stirring . After the addition, heat to reflux and stir, the water separator separates the water produced by the reaction, and GC tracks until the reaction is complete. Zinc chloride was separated, the organic phase was washed with water and saturated sodium bicarbonate, and concentrated to obtain 218.0 g of 4-butyryl resorcinol with a yield of 80.6%.
[0023] Add 90.1g (0.5mol) of 4-butyryl resorcinol to a 1.0L four-necked flask, add 500ml of acetic acid, 10% wet Pd / C (20.0g), under nitrogen protection, heat to 110°C, add 157.7 g ammonium formate (2.5mol), followed by GC until the end of the reaction. Add 2.0L of dichloromethane to the reaction solution, filter and recover Pd / C, wash the filtrate with water, wash with saturated sodium bicarbonate, dry over anhydrous sodium sulfate, and concentrate to ...
Embodiment 2
[0025] Add 165.0 g of resorcinol (1.5 mol) to a 2.0 L four-necked flask, then add 1.0 L of toluene, then add 158.6 g of n-butyric acid (1.8 mol), and add 245.3 g of zinc chloride (1.8 mol) under stirring. After the addition, heat to reflux and stir, the water separator separates the water produced by the reaction, and GC tracks until the reaction is complete. Zinc chloride was separated, the organic phase was washed with water and saturated sodium bicarbonate, and concentrated to obtain 241.5 g of 4-butyryl resorcinol with a yield of 89.3%.
[0026] Add 90.1g (0.5mol) of 4-butyryl resorcinol to a 1.0L autoclave, add 500ml of methanol, 10% wet Pd / C (20.0g), heat to 80°C, and feed hydrogen at a pressure of 1.5MPa , GC tracking to the end of the reaction. The reaction solution was filtered to recover Pd / C, and the filtrate was concentrated to obtain a light brown-red oily liquid, which was recrystallized from dichloromethane and n-hexane to obtain 72.3 g of 4-butylresorcinol, GC...
Embodiment 3
[0028] Add 165.0 g of resorcinol (1.5 mol) to a 2.0 L four-necked flask, then add 1.0 L of xylene, then add 158.6 g of n-butyric acid (1.8 mol), and add 245.3 g of zinc chloride (1.8 mol) under stirring. After the addition, heat to reflux and stir, the water separator separates the water produced by the reaction, and GC tracks until the reaction is complete. Zinc chloride was separated, the organic phase was washed with water and saturated sodium bicarbonate, and concentrated to obtain 232.0 g of 4-butyryl resorcinol with a yield of 85.8%.
[0029] Add 90.1g (0.5mol) of 4-butyryl resorcinol to a 1.0L autoclave, add 500ml of methanol, Raney nickel (20.0g), heat to 80°C, feed hydrogen, pressure 1.5MPa, GC tracking to The reaction is over. The reaction solution was filtered to recover Raney nickel, and the filtrate was concentrated to obtain a light brown-red oily liquid, which was recrystallized from dichloromethane and n-hexane to obtain 54.2 g of 4-butylresorcinol, GC>99.0%, ...
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