Preparation method of amfostine trihydrate
A technology of amifostine trihydrate and amifostine, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve difficulties, large crystal size, high hardness and difficult to crush and other problems, to achieve the effect of improved product stability, moderate particle size and easy crushing
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Embodiment 1
[0015] Take 80.0 g of amifostine trihydrate (water content 20.2%), add 440 ml of purified water to dissolve, the dissolution temperature is 17° C., and the dissolution time is about 5 minutes. After the dissolution is complete, filter and cool the filtrate to 5°C, continue cooling and add 135.0 g of absolute ethanol cooled to 0°C at a constant speed, and dropwise complete in about 10 minutes. After the addition of ethanol, the system temperature was 2.3°C, cooled to 0°C within 1 hour, stirred and crystallized for 1 hour, filtered, washed the filter cake with a small amount of ethanol, and dried in vacuo to obtain 76.5g of white powdery solid, with a yield of 95.6%, and its XRD detection pattern and figure 1 basically the same.
Embodiment 2
[0017] Take 80.0 g of amifostine trihydrate (water content 20.2%), add 440 ml of purified water to dissolve, the dissolution temperature is 17° C., and the dissolution time is about 5 minutes. After the dissolution is complete, filter, and cool the filtrate to 3°C, keep cooling and add 135.0 g of absolute ethanol cooled to 0°C at a uniform speed, and dropwise complete in about 12 minutes. After the addition of ethanol, the temperature of the system was 5.2°C, cooled to 0°C within 1 hour, stirred and crystallized for 1 hour, filtered, washed the filter cake with a small amount of ethanol, and dried in vacuo to obtain 76.6g of white powdery solid, whose XRD detection pattern was consistent with figure 1 basically the same.
Embodiment 3
[0019] Take 80.0 g of amifostine trihydrate (water content 20.2%), add 440 ml of purified water to dissolve, the dissolution temperature is 17° C., and the dissolution time is about 5 minutes. After the dissolution is complete, filter, and cool the filtrate to 5°C, keep cooling and add 135.0 g of absolute ethanol at a constant speed, and the addition is completed in about 15 minutes. After the addition of ethanol, the temperature of the system was 7.2°C, cooled to 0°C within 1 hour, stirring and crystallizing for 0.5 hour, filtering, washing the filter cake with a small amount of ethanol, and drying in vacuo to obtain 76.4g of a white powdery solid, whose XRD detection pattern was consistent with figure 1 basically the same.
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