One-pot synthesis method for 5-bromo-2-chloro-4'-ethoxy diphenylmethane
A technology of ethoxydiphenylmethane and a synthesis method, applied in the field of one-pot synthesis of 5-bromo-2-chloro-4'-ethoxydiphenylmethane, can solve the problems of high consumption of Lewis acid, difficulty in solvent recovery, Complex post-processing and other problems, to achieve the effect of good solvent recovery, low production cost and simple operation
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Embodiment 1
[0016] On the 1L four-necked flask, respectively install a mechanical stirrer, a thermometer, a reflux condenser and a constant pressure dropping funnel, under nitrogen protection, first add 100g of 2-chloro-5-bromobenzoic acid (96%, 0.41mol), 400ml di Chloromethane, stirred, and 68.3 g of thionyl chloride (0.58 mol, 1.4 eq) was added dropwise at room temperature for about 10 minutes. Then it was heated to 70° C. and refluxed for 4 hours, and the reaction was stirred; the reaction solvent and excess thionyl chloride were distilled off under reduced pressure. Add fresh 700ml of anhydrous tetrahydrofuran, 56.1g of phenetole (98%, 0.45mol, 1.1eq.) to the bottle, cool down to -5°C in a cooling bath, and slowly add 68.9g of aluminum trichloride (0.52mol, 1.26eq. ), the temperature is controlled to less than 10°C, and the feeding time is 15 minutes. The reaction was kept at 10° C. for 2 hours, and the residual 2-chloro-5-bromobenzoic acid content detected by HPLC was less than 0.5%...
Embodiment 2
[0020] 100g of 2-chloro-5-bromobenzoic acid (96%, 0.41mol), 400ml of dichloromethane were first added to a 1L four-necked flask, stirred, and 68.3g of thionyl chloride (0.58mol, 1.4 eq), about 20 minutes of time for adding. Then it was heated to 70° C. and refluxed for 3 hours, and the reaction was stirred; the reaction solvent and excess thionyl chloride were distilled off under reduced pressure. Add fresh 700ml of anhydrous tetrahydrofuran to the bottle, 51.1g of phenetole (98%, 0.41mol, 1.0eq), cool down to -5°C in a cold bath, and slowly add 65.6g of aluminum trichloride (0.49mol, 1.2eq) , the temperature is controlled to less than 10°C, and the feeding time is about 10 minutes. The reaction was kept at 10° C. for 3 hours, and the residual 2-chloro-5-bromobenzoic acid content detected by HPLC was less than 0.5%, that is, the reaction was stopped.
[0021] The reaction solution was continued to cool to -10°C, and 22.6g of potassium borohydride (98%, 0.41mol, 1.0eq) was ad...
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