A kind of purification method of brexpiprazole hydrochloride
A purification method, hydrochloride technology, applied in the field of purification of benzo[B]thiophene compounds, can solve problems such as cumbersome operation, unsuitable for large-scale industrial production, difficult to remove by-products, etc.
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Embodiment 1
[0025] To 24 g of crude Brexpiprazole were added 480 ml of ethanol and 24 ml of acetic acid, and the mixture was stirred under reflux to dissolve the crude product. Add 6.5g of hydrochloric acid and cool to 10°C. Heated to reflux again and cooled to 7°C. Crystals were separated and washed with 24 ml of ethanol. The separated crystals were dried at 60°C to obtain 25.3 g of brexpiprazole hydrochloride in a yield of 97.3%.
[0026] Add 20g of Brexpiprazole hydrochloride, 200ml of dimethyl sulfoxide and 1g of activated carbon into the reaction flask, raise the temperature to about 60°C, stir under temperature control for 0.5 hours, filter, transfer the filtrate to the reaction flask, raise the temperature to about 60°C again, and add 200ml Ethyl acetate was stirred under temperature control for 0.5 hours, cooled to room temperature, crystallized for 3 hours, filtered, and the filter cake was dried to obtain 17.8 g of high-purity Brexpiprazole hydrochloride with a yield of 89%. ...
Embodiment 2
[0029] To 24 g of crude Brexpiprazole were added 450 ml of methanol and 20 ml of acetic acid, and the mixture was stirred under reflux to dissolve the crude product. Add 6.7g of hydrochloric acid and cool to 10°C. Heated to reflux again and cooled to 7°C. Crystals were separated and washed with 25 ml of methanol. The separated crystals were dried at 60°C to obtain 25.0 g of brexpiprazole hydrochloride in a yield of 96.2%.
[0030] Add 20g of Brexpiprazole hydrochloride, 220ml of dimethyl sulfoxide and 1.4g of activated carbon into the reaction flask, raise the temperature to about 40°C, stir under temperature control for 0.5 hours, filter, transfer the filtrate to the reaction flask, raise the temperature to about 60°C again, add 66ml of ethanol was stirred under temperature control for 0.5 hours, cooled to 10°C, crystallized for 3 hours, filtered, and the filter cake was dried to obtain 17.2g of high-purity Brexpiprazole hydrochloride with a yield of 86%.
[0031]15 g of B...
Embodiment 3
[0033] To 24 g of crude Brexpiprazole were added 500 ml of tetrahydrofuran and 25 ml of formic acid, and the mixture was stirred under reflux to dissolve the crude product. Add 6.5g of hydrochloric acid and cool to 10°C. Heated to reflux again and cooled to 7°C. Crystals were separated and washed with 25 ml of tetrahydrofuran. The separated crystals were dried at 60°C to obtain 24.8 g of brexpiprazole hydrochloride in a yield of 95.4%.
[0034] Add 20g of Brexpiprazole hydrochloride, 200ml of dimethylformamide and 1.8g of activated carbon into the reaction flask, raise the temperature to about 50°C, stir under temperature control for 0.5 hours, filter, transfer the filtrate to the reaction flask, raise the temperature to about 80°C again, add 250ml of isopropanol was stirred under temperature control for 0.5 hours, cooled to 20°C, crystallized for 3 hours, filtered, and the filter cake was dried to obtain 16.6g of high-purity Brexpiprazole hydrochloride with a yield of 83%. ...
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