Method for preparing 4,4'-di[(2-hydroxyethyl)methylamino]benzophenone
A technology of difluorobenzophenone and dichlorobenzophenone is applied in 4 fields, and can solve the problems of high cost, various types of raw materials, long reaction time, etc., and achieves less three wastes, simple post-processing, and simple reaction process. Effect
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[0021] A preparation method of 4,4'-bis[(2-hydroxyethyl)methylamino]benzophenone, comprising: using 4,4'-dichlorobenzophenone and 4,4'-difluoro At least one of the benzophenones, and N-methyl-2-hydroxyethylamine are dissolved in the reaction solvent (benzene, toluene, xylene or water) together as a raw material, and an acid catalyst (p-toluenesulfonic acid, p-toluenesulfonic acid, Sulfuric acid, phosphomolybdic acid or cationic sulfonic acid resin amberlyst15); heating to 60-140°C for reflux reaction, heat preservation reaction for 12-40h, adding methanol, cooling to 0-5°C for heat preservation and crystallization for 0.5-1.5h, using ice methanol The product was obtained after washing and vacuum drying at 50-55°C.
[0022] Wherein, the molar ratio of the total amount of 4,4'-dichlorobenzophenone and 4,4'-difluorobenzophenone to N-methyl-2-hydroxyethylamine is less than 1:4. The dosage of the catalyst is 0.02-0.5 times of the total mass of 4,4'-dichlorobenzophenone and 4,4'-di...
Embodiment 1
[0024] Preparation before reaction: Make sure the 250ml reaction flask is clean and dry. The reaction flask is equipped with a thermometer (0-200° C.), mechanical stirring, a condenser, and an oil bath.
[0025] Add 31.61g of 4,4'-dichlorobenzophenone, 38g of N-methyl-2-hydroxyethylamine, 140g of xylene and 1g of p-toluenesulfonic acid monowater into the reaction flask, start stirring, and heat To reflux temperature (about 140°C), keep warm for 12h.
[0026] After the reaction is complete, turn off the heating, cool down the reaction flask to about 70°C, vacuumize and recover the solvent until no solvent is evaporated. 120 g of methanol was added thereto, the temperature was continued to drop to 0° C., and the mixture was kept stirring for 1 h.
[0027] After filtering, the reaction flask was washed with 30 g of ice methanol, and the filter cake was rinsed. The filter cake was dried under vacuum at 50-55°C until no weight loss ceased. Obtained product: about 30.3g, content...
Embodiment 2
[0029] Preparation before reaction: Make sure the 250ml reaction flask is clean and dry. The reaction flask is equipped with a thermometer (0-200° C.), mechanical stirring, a condenser, and an oil bath.
[0030] Add 31.61g of 4,4'-dichlorobenzophenone, 50g of N-methyl-2-hydroxyethylamine, 100g of benzene and 10g of cationic sulfonic acid resin amberlyst15 into the reaction flask, start stirring, and heat to 60 ℃. Keep warm for 40 hours.
[0031] After the reaction was completed, the catalyst was filtered out. Benzene was recovered under normal pressure until no material was evaporated, and 120 g of methanol was added to the residual liquid, and the temperature was further lowered to 0°C, and kept stirring for 1 h.
[0032] After filtering, the reaction flask was washed with 30 g of ice methanol, and the filter cake was rinsed. The filter cake was dried under vacuum at 50-55°C until no weight loss ceased. Obtained product: about 34g, content: 98.1%, yield: 82%.
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