A kind of synthetic method of trihydrate 3-aminopropylamine ethylthiophosphoric acid
A technology of aminopropylamine ethylthiophosphoric acid and its synthesis method, which is applied in the field of synthesis of trihydrate 3-aminopropylamineethylthiophosphoric acid to achieve good biocompatibility, high purity and high purity of the crude product Effect
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[0040] Example 1 Synthesis process of amifostine of the present invention
[0041] a. Add sodium thiophosphate dodecahydrate (10.0 g, 25.2 mmol) and 25 ml of distilled water to a flask equipped with an internal temperature thermometer, stir and suspend, and use an ice water bath outside. First add N-(2-bromoethyl)-1,3-propanediamine dihydrobromide (9.5g, 27.7mmol) to obtain a light brown suspension system, and then add polyethylene glycol 400 that is PEG400 ( 10g), after stirring evenly, remove the ice-water bath and keep stirring at 5-10°C for reaction. During the reaction, the reaction system first turned into a light brown clear solution, and then turned into an off-white turbid system again.
[0042] b. After 24 hours of reaction, add 163ml of concentrated ammonia-methanol mixture (volume ratio 1 / 29) to the stirred reaction material at room temperature, and a white solid can be seen in the bottle. After stirring for about 10 minutes, stand still at 4°C for crystallization. F...
Example Embodiment
[0043] Example 2 Synthesis process of amifostine of the present invention
[0044] First, the crude amifostine was synthesized according to the process of Example 1, and then refined by the following operations:
[0045] One-time refining: Take 1g of the above crude product, add 10ml of 5% volume ethanol solution to dissolve, add 0.02g activated carbon and 1.0g 201×7 type strong acid anion exchange resin, stir in 30℃ oil bath for 10min, filter under normal pressure, and water The phase was kept in a 30°C oil bath with stirring and 4ml of 99.5% ethanol was added dropwise, and then the bath temperature was gradually reduced from 30°C to room temperature. At this time, a large amount of white solid has been precipitated, and then left standing at 4°C for 2h, suction filtration, and vacuum drying at 30°C to obtain 0.78g of a white primary refined product with a yield of 78% and a content determined by HPLC of about 98%.
[0046] Secondary refining: take 1g of the above-mentioned primary...
Example Embodiment
[0047] Example 3 Screening test of different conditions for the synthesis process of amifostine of the present invention
[0048] The following table is the experimental results obtained when preparing crude amifostine with different ingredient ratios and reaction temperatures according to the operation process of step a in Example 1 (the method of step b is the same)
[0049] Table 1
[0050]
[0051] It can be seen from Table 1 that the dosage ratio of water and PEG has an important influence on the yield and purity of the reaction: when the weight ratio of sodium salt to bromide salt is 1:0.8-1.3, the weight ratio of water to PEG is 4 :1~1:3, the product yield is above 54%, and the purity is higher than 73%; when the weight ratio of water to PEG is 4:1~1.6:1, the product yield is above 83% , And the purity is higher than 87%, indicating that the conditions are better than the existing pure water reaction system (such as Li Jiaming, etc., Anhui Chemical Industry, 2000, 2:17-18); w...
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