Method for synthesizing light-sensitive material 2,3,4,4'-Tetrahydroxybenzophenone
A technology of tetrahydroxybenzophenone and photosensitive materials, applied in the direction of condensation preparation of carbonyl compounds, organic chemistry, etc., can solve the problems of high residual metal ion content of products, failure to meet the requirements of the microelectronics industry, and difficulty in industrialized large-scale production. Achieve the effects of good crystallization, small environmental impact, and improved reaction speed
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Embodiment 1
[0016] Pyrogallic acid (0.01mol, 126g), p-hydroxybenzoic acid (0.0105mol, 152g) were mixed with 1000ml of 1,1,2,2-tetrachloroethane, magnetically stirred, and boron trifluoride ether solution was slowly added dropwise ( 12%) 300mL, after the addition, the temperature was raised to 100°C for 2h, and yellow crystals were precipitated, and after cooling, filtered, the filter cake was washed twice with 5% sodium carbonate solution and water respectively, the crystals were collected, and washed with 900ml of 35% ethanol Dissolved, recrystallized at 0-10°C, centrifugally filtered, washed with distilled water to obtain 172.3 g of light yellow needle-like crystal product 2,3,4,4'-tetrahydroxybenzophenone, yield 62%, HPIC analysis result content 99.6 %.
Embodiment 2
[0018] Mix pyrogallic acid (0.01mol, 126g), p-hydroxybenzoic acid (0.0105mol, 152g) with 1000ml of 1,1,2,2-tetrachloroethane, stir magnetically, and use concentrated sulfuric acid, sodium bisulfate, chlorine Zinc chloride replaces boron trifluoride diethyl ether as a catalyst, and reacts under similar conditions in Method 1, but does not obtain the desired product.
Embodiment 3
[0020] Pyrogallic acid (252g, 0.02mol), p-hydroxybenzoic acid (304g, 0.021mol) and anhydrous ZnCl 2 (410g, 0.03mol) mixed, magnetically stirred, slowly added 2000ml of 1,2-dichloroethane, heated to 50°C, reacted for 8h, cooled to room temperature, the reaction mixture was slowly poured into ice water, and fully stirred, and stood for 30mim , to separate out solids, filter, and the filter cake is washed twice with 5% sodium carbonate solution and distilled water respectively, collect the crystals, recrystallize with 2200ml of 35% ethanol, centrifugally filter, wash with distilled water to obtain 459.3g of light yellow crystals, the yield 82.6%, the HPIC analysis result content is 99.5%.
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