Temozolomide refining process
A technology of temozolomide and a purification method, which is applied in the purification field of antitumor drug temozolomide, can solve the problems of complicated process, high cost and the like, and achieves the effects of simple operation, good effect and cost reduction.
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Embodiment 1
[0037] 552 g of dimethyl sulfoxide was added into a three-necked flask, and 100 g of crude temozolomide was added under stirring conditions. Raise the temperature to complete dissolution, add an appropriate amount of activated carbon to decolorize for 30 minutes, heat filter, transfer the filtrate to a clean container, and cool the mother liquor at room temperature to separate the essence, about (t=4h). Suction filter the mother liquor, and filter the cake with anhydrous Wash with 1.2kg of ethanol, 400g each time, three times, and then drain. Transfer the filter cake to another clean container, add 1.2kg of absolute ethanol, heat to reflux for 10-15 minutes, perform hot suction filtration, wash with 1.2kg of absolute ethanol three times, 400g each time, and then drain. After the product is recovered from the filtrate, ethanol is recovered. The filter cake was vacuum-dried for 12 hours at room temperature, and 83.5 g was obtained after discharge, with a yield of 83.5%. The co...
Embodiment 2
[0039] 828 g of dimethyl sulfoxide was added into a three-necked flask, and 150 g of crude product temozolomide was added under stirring conditions. Raise the temperature to complete dissolution, add an appropriate amount of activated carbon to decolorize for 30 minutes, transfer the filtrate to a clean container, and cool the mother liquor at room temperature to separate the essence, about (t=4h). Suction filter the mother liquor, and use 1.8kg of absolute ethanol for the filter cake Wash, 600g each time, wash three times, and then drain. Transfer the filter cake to another clean container, add 1.8kg of absolute ethanol, heat to reflux for 10-15 minutes, carry out hot suction filtration, wash with 1.8kg of absolute ethanol three times, 600g each time, and then drain. After the product is recovered from the filtrate, ethanol is recovered. The filter cake was vacuum-dried for 12 hours at room temperature, and 123 g was obtained after discharging, with a yield of 82%. The colo...
Embodiment 3
[0041] 662.4 kg of dimethyl sulfoxide was added into a three-necked flask, and 120 g of crude product temozolomide was added under stirring conditions. Raise the temperature to complete dissolution, add an appropriate amount of activated carbon to decolorize for 30 minutes, heat filter, transfer the filtrate to a clean container, and cool the mother liquor at room temperature to separate the essence, about (t=4h). Suction filter the mother liquor, and filter the cake with anhydrous Wash with 480g of ethanol, wash three times, and then drain. Transfer the filter cake to another clean container, add 480g of absolute ethanol, heat to reflux for 10-15 minutes, carry out hot suction filtration, wash with 480g of absolute ethanol three times, and then suck dry. After the product is recovered from the filtrate, ethanol is recovered. The filter cake was vacuum-dried for 12 hours at room temperature, and 99 g was obtained after discharge, with a yield of 82.5%. The color of the produ...
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