A kind of refining method of pralatrexate intermediate
A refining method, the technology of pralatrexate, which is applied in the field of medicine, can solve the problems that there is no refining method for the finished product of pralatrexate, and achieve the effects of cost saving, process simplification and yield improvement
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Embodiment 1
[0020] Add 15g of crude pralatrexate intermediate PLQS-6 and 225ml of methanol into a 500ml three-necked flask, heat until completely dissolved, add 4.5g of activated carbon to decolorize for 0.5h while it is hot, filter while it is hot, cool the filtrate to 0-5°C and stir Crystallize, filter, rinse the filter cake with methanol, and dry to obtain 13.9 g of the refined product of pralatrexate intermediate PLQS-6. The purity is 99.89%, and the yield is 92.7%.
Embodiment 2
[0022] Add 15g of the crude product of pralatrexate intermediate PLQS-6 and 75ml of methanol into a 500ml three-neck flask, heat until completely dissolved, add 1.5g of activated carbon to decolorize for 0.5h while it is hot, filter while it is hot, cool the filtrate to 0-5°C and stir Crystallize, filter, rinse the filter cake with methanol, and dry to obtain 14.0 g of the refined product of pralatrexate intermediate PLQS-6. The purity is 99.83%, and the yield is 93.3%.
Embodiment 3
[0024] Add 15g of crude pralatrexate intermediate PLQS-6 and 300ml of methanol into a 500ml three-neck flask, heat until completely dissolved, add 6.0g of activated carbon to decolorize for 0.5h while it is hot, filter while it is hot, cool the filtrate to 0-5°C and stir Crystallize, filter, rinse the filter cake with methanol, and dry to obtain 13.4 g of the refined product of pralatrexate intermediate PLQS-6. The purity is 99.85%, and the yield is 89.3%.
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