Preparation method of pralatrexate
A technology of crystallization and reaction solvent, applied in the field of preparation of pralatrexate, can solve the problems of increasing impurities, failing to meet refining requirements, no refining effect, etc., achieving simple operation, high purity and yield, and reducing product The effect of quality
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Embodiment 1
[0029] Add 20g of PLQS-6 and 100ml of acetone into a 2L three-necked flask and stir. When the temperature is controlled at about 10°C, the bottle becomes a suspension. Start adding 15ml of 1.0mol / L sodium hydroxide aqueous solution dropwise, and control the rate of addition so that the temperature of the reaction flask is 10~13°C, after the dropwise addition is completed, keep stirring for 2 hours, continue to add 15ml of 1.0mol / L sodium hydroxide aqueous solution dropwise, repeat the above operation until all the 91ml of sodium hydroxide aqueous solution is added dropwise, continue to keep stirring for 2 hours, and the reaction solution is clear. Sampling for HPLC detection; the reaction is complete, put the three-neck bottle in a cold bath to cool down to 0-5°C, add 720ml of absolute ethanol dropwise, at this time, a yellow solid precipitates, after the dropwise addition, continue to keep stirring for 1 hour, filter, and add to the filter cake Dissolve in 200ml of purified wa...
Embodiment 2
[0031] Add 20g of PLQS-6 and 200ml of dioxane into a 2L three-neck flask and stir. When the temperature is controlled at about 10°C, the bottle becomes a suspension. Start to add 15ml of 1.0mol / L sodium carbonate aqueous solution dropwise, and control the dropping speed to make the reaction bottle The temperature is 10-13°C. After the dropwise addition is completed, keep stirring for 2 hours, continue to add 15ml of 1.0mol / L sodium carbonate aqueous solution dropwise, repeat the above operation until all the 91ml of sodium carbonate aqueous solution is added dropwise, continue to keep warm and stir for 4 hours, and the reaction solution is clear. Sampling for HPLC detection; the reaction is complete, put the three-neck bottle in a cold bath to cool down to 0-5°C, add 720ml of absolute ethanol dropwise, at this time, a yellow solid precipitates, after the dropwise addition, continue to keep stirring for 1 hour, filter, and add to the filter cake Dissolve in 200ml of purified wat...
Embodiment 3
[0033] Add 20g of PLQS-6 and 60ml of acetone into a 2L three-necked flask and stir. When the temperature is controlled at about 10°C, the bottle becomes a suspension. Start to add 15ml of 1.0mol / L sodium hydroxide aqueous solution dropwise, and control the rate of addition so that the temperature of the reaction flask is 10~13°C, after the dropwise addition is completed, keep stirring for 2 hours, continue to add 15ml of 1.0mol / L sodium hydroxide aqueous solution dropwise, repeat the above operation until all the 91ml of sodium hydroxide aqueous solution is added dropwise, continue to keep stirring for 2 hours, and the reaction solution is clear. Sampling for HPLC detection; the reaction is complete, put the three-neck bottle in a cold bath to cool down to 0-5°C, add 720ml of acetone dropwise, at this time, a yellow solid precipitates, after the dropwise addition, continue to keep stirring for 1 hour, filter, add 200ml of filter cake to purify Dissolve in water, stir with 200ml...
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