A kind of method for preparing 1,1'-bi-2-naphthol by inorganic base-assisted catalysis
A technology of catalytic preparation and inorganic base, which is applied in the chemical industry, can solve problems such as difficulties, and achieve the effects of reducing production costs, mild conditions, and easy recovery
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Embodiment 1
[0032] 45g of 2-naphthol, 333.5g of 1,2-dichloroethane, 150g of water, 0.31g of solid CuCl and 0.125g of NaOH were added to a 500ml four-necked flask equipped with heating, stirring, thermometer and reflux condenser, and then Heating and controlling the temperature to 50~80℃, feeding oxygen with a flow rate of 100~500ml / min for oxidation, the reaction was carried out for 7 hours, the reaction was stopped, and the reaction mixture solution was cooled and filtered 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 pulped and washed with deionized water, filtered and washed to a solid pH of 6 to 7, and dried to obtain 40.6 g of 1,1'-bi-2-naphthol washed crude product. The washed crude product was recrystallized to obtain 31.6 g of 1,1'-bi-2-naphthol product, the liquid chromatographic purity after drying was 99.2%, and the melting point was 216.4-217.7°C.
Embodiment 2
[0034] 45g of 2-naphthol, 333.5g of 1,2-dichloroethane, 150g of water, 0.31g of solid CuCl and 0.175g of KOH were added to a 500ml four-necked flask equipped with heating, stirring, thermometer and reflux condenser, and then Heating to 50°C, and controlling the temperature to 50-80°C, feeding oxygen with a flow rate of 100-500ml / min for oxidation, the reaction was carried out for 7 hours, the reaction was stopped, and the reaction mixture solution was cooled and filtered to obtain 1,1'-linked- The 2-naphthol crude product has a reaction yield of 89.8%, and the filtrate is distilled to recover the solvent for recycling. The crude product was pulped and washed with deionized water, filtered, and washed to a solid pH of 6 to 7. After drying, 40.4 g of 1,1'-bi-2-naphthol washed crude product was obtained. The washed crude product was recrystallized to obtain 30.9 g of 1,1'-bi-2-naphthol product. After drying, the liquid chromatography purity was 99.1%, and the melting point was 21...
Embodiment 3
[0036]In a 500ml four-necked flask equipped with heating, stirring, thermometer and reflux condenser, add 2-naphthol 45g, 1,2-dichloroethane 333.5g, 150g water, solid CuCl 0.31g and Na 2 CO 3 0.331g, then heated to 50 ℃, and the temperature was controlled at 50-80 ℃, and oxygen with a flow rate of 100-500ml / min was introduced for oxidation, the reaction was carried out for 7 hours, the reaction was stopped, and the reaction mixture solution was cooled and filtered to obtain 1,1 '-bi-2-naphthol crude product, the reaction yield is 88.9%, and the filtrate is distilled to recover the solvent for recycling. The crude product was pulped and washed with deionized water, filtered, and washed to a solid pH of 6 to 7. After drying, 40.0 g of 1,1'-bi-2-naphthol washed crude product was obtained. The washed crude product was recrystallized to obtain 29 g 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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