Polythiol-substituted aryl compound and preparation method thereof
A compound and aryl technology, applied in the field of intermediates and preparation of polysulfonic acid substituted aryl compounds, can solve the problems of increasing preparation cost, higher requirements on equipment for sulfonation conditions, increasing production cost, etc., so as to reduce preparation cost , The effect of low equipment requirements and easy operation
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Embodiment 1
[0053] Synthesis of bis(4-fluoro-3,5-dimercaptophenyl)methanone: (1) bromination reaction: 10.5g (0.048mol) of 4,4'-difluoro-benzophenone was dissolved in 20mL acetic acid and 100mL of concentrated sulfuric acid, stirred at room temperature, dissolved completely after 20min; reduce the temperature of the mixture to between 0 and -5°C. Weigh 36 g (0.126 mol) of dibromohydantoin and add it to the above mixture in batches. After the addition is complete, keep warm at about 0°C and stir for 2 hours, then slowly raise the temperature to 45°C for 4 hours, and detect the product formation by HPLC. After the reaction, the reaction solution was slowly poured into 1 kg of ice water, stirred, filtered, and washed with water for 3*300 mL to obtain bis(3,5-dibromo-4-fluorophenyl)methanone as a white solid. After drying in a vacuum oven for 2 hours, the crystals were dissolved in tetrahydrofuran to obtain 19.5 g of colorless needle-like crystals. The purity measured by HPLC was 93%, and the...
Embodiment 2
[0059] Synthesis of bis(4-fluoro-3,5-dimercaptophenyl)methanone: (1) bromination reaction: 10.5g (0.048mol) of 4,4'-difluoro-benzophenone was dissolved in 20mL acetic acid and 100mL of concentrated sulfuric acid, stirred at room temperature, and dissolved completely after 20 minutes; reduce the temperature of the mixture to between 5 and 0°C. Take 22.7g (0.126mol) of liquid bromine and add it dropwise to the above mixed solution in batches. After the addition is complete, keep warm at about 0°C and stir for 2h, slowly raise the temperature to 45°C for 4h, and detect the product formation by HPLC. After the reaction, the reaction solution was slowly poured into 1 kg of ice water, stirred, filtered, and washed with water for 3*300 mL to obtain bis(3,5-dibromo-4-fluorophenyl)methanone as a white solid. After drying in a vacuum oven for 2 hours, the crystals were dissolved in tetrahydrofuran to obtain 19.5 g of colorless needle-like crystals, the purity of which was 93% as measure...
Embodiment 3
[0061] Synthesis of bis(4-fluoro-3,5-dimercaptophenyl)methanone: (1) bromination reaction: 10.5g (0.048mol) of 4,4'-difluoro-benzophenone was dissolved in 200mL tetrahydrofuran , stir and dissolve completely at room temperature; reduce the temperature of the mixture to between 0 and -3°C. Weigh 44.8g (0.25mol) of N-bromo-succinimide and add it to the above mixture in batches. After the addition is complete, keep warm at about 0°C and stir for 2h, then slowly raise the temperature to 45°C for 4h, and detect the product formation by HPLC. After the reaction, the reaction solution was slowly poured into 1 kg of ice water, stirred, filtered, and washed with water for 3*300 mL to obtain bis(3,5-dibromo-4-fluorophenyl)methanone as a white solid. After drying in a vacuum oven for 2 h, the crystals were dissolved in tetrahydrofuran to obtain 16.1 g of colorless needle crystals. (2) Substitution reaction: Dissolve 5.3g (0.01mol) of bis(3,5-dibromo-4-fluorophenyl)methanone in 0.2L tolu...
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