Method for preparing high-purity fosinopril sodium
A fosinopril sodium, high-purity technology is applied in the field of preparation of fosinopril sodium compounds, can solve the problems of low purity, unsuitable for industrial production, low yield of fosinopril sodium and the like, and achieves product yield and the effect of high purity and simple method
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no. 1 example
[0014] Put fosinopril sodium crude product 5g (purity is 95.5%) in reaction bottle, add 5% hydrochloric acid solution slowly, and stir, measure system pH value, when pH=4, add trimethyl phosphate 10g, fully Stir, then stand still for 30min, collect the organic phase, then continue to add 5g of trimethyl phosphate in the water phase, repeat the above operation 3 times, collect all the organic phase, add a 5% NaOH solution, stir well, and then slowly heat , control the temperature at 50°C and keep it for 5 minutes, a large amount of solids are produced, the system is cooled to room temperature, filtered to obtain a filter cake, washed with trimethyl phosphate, and dried in vacuum to obtain high-purity fosinopril sodium, collected The yield is 95.8%, and the purity is greater than 99.8%.
no. 2 example
[0016] Put 8 g of fosinopril sodium crude product (purity is 95.5%) in the reaction bottle, slowly add 10% sulfuric acid solution, and stir, measure the pH value of the system, when pH=3, add 12 g of triethyl phosphate, Stir fully, then stand still for 20min, collect the organic phase, then continue to add 8g triethyl phosphate in the water phase, repeat the above operation 3 times, collect all the organic phases, add a 10% sodium bicarbonate solution, stir well, and then Heat slowly, control the temperature at 80°C, and keep it for 10 minutes. A large amount of solids are produced. Cool the system to room temperature and filter to obtain a filter cake. Wash the filter cake with triethyl phosphate and dry it in vacuum to obtain high-purity fosinopril Sodium, the yield is 97.1%, and the purity is greater than 99.8%.
no. 3 example
[0018] Put 10g of fosinopril sodium crude product (purity is 95.5%) into the reaction bottle, slowly add 20% concentration of phosphoric acid solution, and stir, measure the pH value of the system, when pH=4, add diethyl ethyl phosphate 20g, fully stirred, then stand still for 10min, collect the organic phase, then continue to add 12g diethyl ethyl phosphate in the water phase, repeat the above operation 5 times, collect all the organic phases, add a concentration of 30% sodium hydrogen phosphate solution, Stir well, then heat slowly, control the temperature at 150°C, keep it for 30 minutes, a large amount of solids are produced, cool the system to room temperature, filter to obtain a filter cake, wash the filter cake with diethyl ethyl phosphate, and dry it in vacuum to obtain high Purity of fosinopril sodium, yield 97.9%, purity greater than 99.8%.
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