A method for synthesizing intermediate impurities of antigout drug febuxostat and applications of the synthesized impurities
A technology for febuxostat and an anti-gout drug, applied in the field of medicine, can solve problems such as impurities that cannot meet identification standards, and achieve the effects of simple synthesis method and high purity
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Embodiment 1
[0036] Synthesis of Impurity A
[0037] In a 50mL three-necked flask equipped with a magnetic stirrer, a condenser and a thermometer, add 5.00 g (32.63 mmol) of 4-hydroxythiobenzamide, 40 g of absolute ethanol, and 3.60 g (39.16 mmol) of chloroacetone at 75 ° C The reaction was stirred for 2 hours (monitored by TLC). After the reaction stopped, the temperature was lowered to 20-25° C., filtered, and the filter cake was washed with absolute ethanol to obtain 6.18 g of intermediate 1 as a white solid, HPLC: 98.25%, yield: 99.03%;
[0038] In a 100mL three-necked flask equipped with a magnetic stirrer, a condenser and a thermometer, add 10.00g (52.28mmol) of intermediate 1 and 60g of TFA and stir and mix. ℃, react at the same temperature for 5 hours, after the reaction stops, cool down to 20-25℃, add 100g of purified water, 100g of dichloromethane for extraction, after separation, the organic phase is sequentially washed with saturated NaHCO 3 Solution washing, saturated brine w...
Embodiment 2
[0045] Synthesis of Impurity A
[0046] In a 50mL three-necked flask equipped with a magnetic stirrer, a condenser and a thermometer, add 10.00 g (65.26 mmol) of 4-hydroxythiobenzamide, 80 g of absolute ethanol, and 7.20 g (78.32 mmol) of chloroacetone at 78 ° C The reaction was stirred for 3 hours (monitored by TLC). After the reaction stopped, the temperature was lowered to room temperature, filtered, and the filter cake was washed with absolute ethanol to obtain 11.18 g of intermediate 1 as a white solid, yield: 89.58%;
[0047] In a 100mL three-necked flask equipped with a magnetic stirrer, a condenser and a thermometer, add 15.00g (78.43mmol) of Intermediate 1 and 90g of TFA to stir and mix, add 15.83g of HMTA (109.79mmol) after clarification, and heat up to 100°C. React at the same temperature for 6 hours. After the reaction stops, cool down to 25°C, add 100g of purified water, and extract with 100g of dichloromethane. After liquid separation, the organic phase is sequen...
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