Preparation method of oxygen bleaching activator tribasic copper chloride (TBCC)
A solvent and chloride technology, applied in the field of chemical synthesis, can solve the problems of complex synthesis process, expensive raw materials, low product yield, etc., and achieve the effect of simple synthesis process, environmental friendliness and low production cost
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example 1
[0044] Synthesis of 14-bromomethylbenzoic acid (2)
[0045] Add 13.62 g (0.10 mol) of 4-methylbenzoic acid, 17.82 g (0.10 mol) of NBS, 1.99 g of BPO, and 120 mL of carbon tetrachloride into a 250 mL three-necked flask. After fully stirring at room temperature, the reaction system was heated to reflux state and reacted for 4 hours. After the reaction, the reaction system was cooled with an ice-water bath, and a white solid was obtained by suction filtration. The solid was washed with water, filtered by suction, and dried to obtain 17.96 g of a white solid of 4-bromomethylbenzoic acid, with a yield of 84%. m.p.225-227°C.
[0046] Synthesis of 24-Hydroxymethylbenzoic Acid (3)
[0047] Add 8.60g (0.04mol) of 4-bromomethylbenzoic acid, 10.50mL of concentrated hydrochloric acid and 90mL of water into a 250mL three-necked flask, stir evenly, heat up to 100°C, and react for 4h. After the reaction was finished, it was cooled to room temperature, and then cooled in an ice-water bath,...
example 2
[0053] Synthesis of 14-bromomethylbenzoic acid (2)
[0054] Add 13.66 g (0.10 mol) of 4-methylbenzoic acid, 21.36 g (0.12 mol) of NBS, 1.95 g of BPO, and 120 mL of carbon tetrachloride into a 250 mL three-necked flask. After fully stirring at room temperature, the reaction system was heated to reflux state and reacted for 3 hours. After the reaction is over. The reaction system was cooled with an ice-water bath, and a white solid was obtained by suction filtration. The solid was washed thoroughly with water, filtered by suction, and dried to obtain 17.85 g of a white solid of 4-bromomethylbenzoic acid, with a yield of 83%. m.p.225-227°C.
[0055] Synthesis of 24-Hydroxymethylbenzoic Acid (3)
[0056] Add 9.15g of 4-bromomethylbenzoic acid (0.43×10 -1 mol), concentrated hydrochloric acid 15mL and water 90mL, after stirring evenly, the temperature was raised to 100°C for 6h. After the reaction, the system was cooled to room temperature, and then cooled with an ice-water bat...
example 3
[0062] Synthesis of 14-bromomethylbenzoic acid (2)
[0063] Add 13.64 g (0.10 mol) of 4-methylbenzoic acid, 17.81 g (0.10 mol) of NBS, 1.95 g of BPO, and 120 mL of carbon tetrachloride into a 250 mL three-necked flask. After fully stirring at room temperature, the reaction system was heated to reflux state and reacted for 4 hours. After the reaction, the reaction system was cooled with an ice-water bath, and a white solid was obtained by suction filtration. The solid was washed with water, filtered by suction, and dried to obtain 19.16 g of a white solid of 4-bromomethylbenzoic acid, with a yield of 90%. m.p.225-227°C.
[0064] Synthesis of 24-Hydroxymethylbenzoic Acid (3)
[0065] Add 8.60g (0.04mol) of 4-bromomethylbenzoic acid, 10mL of concentrated hydrochloric acid and 90mL of water into a 250mL three-necked flask, mix well, heat up to 100°C, and react for 4h. After the reaction was finished, cool to room temperature and cool in an ice-water bath. A large amount of whit...
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