Impurities obtained from the preparation of pidotimod ethyl ester and its quality detection method
A quality detection method, the technology of Domodex ethyl ester, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems such as impurities, and achieve accurate and efficient results
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Embodiment 1
[0027] In the quality detection method for the preparation of pidotimod ethyl ester in this embodiment, L-thioproline ethyl ester hydrochloride (500g, 2.53mol) and 1500g of dichloromethane were added to a 3L reaction flask, cooled to 0~ 5°C, dropwise add 20% sodium hydroxide solution (531.16g, 2.66mol), keep the internal temperature at 0-10°C during the dropwise addition, after the dropwise addition, the pH value is 8-9, continue to stir for 5min, and separate the phases , wash the organic phase with 500g of saturated sodium chloride, then add 500g of anhydrous sodium sulfate to the organic phase to dry for 1-2 h, filter, wash the filter cake with 500g of dichloromethane, and pour the filtrate into another 5L reaction flask , add L-pyroglutamic acid (326.56g, 2.53mol), stir for 30min, cool to 0-5°C, add dropwise a mixed solution of dicyclohexylcarbodiimide (521.88g, 2.53mol) and dichloromethane 1000g , keep the temperature at 0-10°C during the dropwise addition, return to 15-2...
Embodiment 2
[0039] The quality detection method of the preparation pidotimod ethyl ester of the present embodiment, the rest is the same as embodiment 1, the difference is: dicyclohexylcarbodiimide adopts the N of equimolar amount, N'-diisopropyl Instead of carbodiimide, the pH value of sodium dihydrogen phosphate phosphoric acid solution and methanol is 2.5, wherein the volume ratio of methanol to sodium dihydrogen phosphate phosphoric acid solution is 60:40. The reaction product was detected by high performance liquid chromatography. The peak area of compound A was 5.1123%, and the peak area of compound B was 1.8637%, which met the requirements.
Embodiment 3
[0041] The quality detection method of the preparation pidotimod ethyl ester of the present embodiment, all the other parts are identical with embodiment 1, difference is: dicyclohexylcarbodiimide adopts the 1-(3-dimethylaminopropane of equimolar amount) Base)-3-ethylcarbodiimide hydrochloride instead, the pH value of sodium dihydrogen phosphate phosphoric acid solution and methanol is 3.5, wherein the volume ratio of methanol to sodium dihydrogen phosphate phosphoric acid solution is 80:20. The reaction product was detected by high performance liquid chromatography. The peak area of compound A was 5.9822%, and the peak area of compound B was 1.5061%, which met the requirements.
[0042]The reagents used in the present invention are all purchased products unless otherwise specified, and the concentrations are all chemically pure.
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