Method for preparing 1, 1'-bi-2-naphthol through inorganic base assisted catalysis
A technology of catalytic preparation and inorganic base, which is applied in the field of chemical industry, can solve problems such as difficulties, and achieve the effects of reducing preparation costs, mild conditions, and accelerating the reaction rate
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Embodiment 1
[0032] Add 45g of 2-naphthol, 333.5g of 1,2-dichloroethane, 150g of water, 0.31g of solid CuCl and 0.125g of NaOH in a 500ml four-neck flask with heating, stirring, thermometer, and reflux condenser device, and then Heat and control the temperature to 50-80°C, pass in oxygen at a flow rate of 100-500ml / min to oxidize, react for 7 hours, stop the reaction, cool down the reaction mixture solution, and filter to obtain 1,1'-bi-2-naphthol The crude product has a reaction yield of 90.2%, and the filtrate is distilled to recover the solvent for recycling. The crude product was beaten and washed with deionized water, filtered and washed until the solid pH = 6-7, and dried to obtain 40.6 g of the crude product washed with water of 1,1'-bi-2-naphthol. The crude product washed with water was recrystallized to obtain 31.6g of 1,1'-bi-2-naphthol product, the purity of liquid chromatography after drying was 99.2%, and the melting point was 216.4-217.7°C.
Embodiment 2
[0034] Add 45g of 2-naphthol, 333.5g of 1,2-dichloroethane, 150g of water, 0.31g of solid CuCl and 0.175g of KOH in a 500ml four-neck flask with heating, stirring, thermometer, and reflux condenser device, and then Heating to 50°C, and controlling the temperature at 50-80°C, passing in oxygen at a flow rate of 100-500ml / min for oxidation, the reaction was carried out for 7 hours, and the reaction was stopped, and the reaction mixed solution was cooled and filtered to obtain 1,1'-linked- The crude product of 2-naphthol has a reaction yield of 89.8%, and the filtrate is distilled to recover the solvent for recycling. The crude product was beaten and washed with deionized water, filtered, and washed until the pH of the solid was 6-7. After drying, 40.4 g of the crude 1,1’-bi-2-naphthol was obtained. The crude product washed with water was recrystallized to obtain 30.9 g of 1,1'-bi-2-naphthol product. The purity of liquid chromatography after drying was 99.1%, and the melting poin...
Embodiment 3
[0036]Add 45g of 2-naphthol, 333.5g of 1,2-dichloroethane, 150g of water, 0.31g of solid CuCl and Na 2 CO 3 0.331g, then heated to 50°C, and controlled at 50-80°C, and oxidized with oxygen at a flow rate of 100-500ml / min. The reaction was carried out for 7 hours, and the reaction was stopped. The reaction mixture solution was cooled and filtered to obtain 1,1 The crude product of '-linked-2-naphthol has a reaction yield of 88.9%, and the filtrate is distilled to recover the solvent for recycling. The crude product was beaten and washed with deionized water, filtered, and washed until the solid pH = 6-7. After drying, 40.0 g of the crude 1,1'-bi-2-naphthol was obtained. The crude product washed with water was recrystallized to obtain 29g of 1,1'-bi-2-naphthol product. After drying, the liquid chromatographic purity was 99.1%, and the melting point was 216.2-217.8°C.
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