Quality control method of D-(+)-alpha-(2-thiofuran ethylamino)-alpha-(2-chlorphenyl) methyl acetate or salt thereof and application of D-(+)-alpha-(2-thiofuran ethylamino)-alpha-(2-chlorphenyl) methyl acetate or salt thereof in clopidogrel production
A thiopheneethylamine-based, clopidogrel technology, applied in the production of clopidogrel, in the field of optical purity determination of a clopidogrel intermediate D--α--α-methyl acetate or a salt thereof, can solve the problem of There are many optical impurities, which cannot accurately reflect the optical purity of the intermediates, the situation of impurities and the content of each impurity, so as to achieve the effect of good separation effect.
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Embodiment 1
[0061] Methodology Validation
[0062] Chromatographic conditions
[0063] Mobile phase: V 正己烷 :V 乙醇 :V 甲醇 =80:15:5;
[0064] Detection wavelength: 220nm;
[0065] Flow rate: 1.0mL / min;
[0066] Column temperature: room temperature;
[0067] Injection volume: 20μL
[0068] 1. System adaptability
[0069] Prepare the racemic α-(2-thienylethylamino)-α-(2-chlorophenyl)acetic acid methyl ester hydrochloride solution with a concentration of 0.2mg / mL, and obtain the following chromatographic conditions according to the above-mentioned chromatographic conditions: figure 1 The spectrum shown was repeated 5 times and calculated from the results: the RSD (relative standard deviation) of the retention time of compound I was 0.1%, and the RSD of the peak area was 0.7%; the RSD of the retention time of compound II was 0.05%, and the peak area The RSD of the compound was 0.5%, the compound I and the compound II achieved baseline separation, the resolution was 7.5, and the ratio of ...
Embodiment 2
[0079] Chromatographic conditions
[0080] Mobile phase: V 正己烷 :V 乙醇 :V 甲醇 =80:15:5;
[0081] Detection wavelength: 220nm;
[0082] Flow rate: 1.0mL / min;
[0083] Column temperature: room temperature;
[0084] Injection volume: 20μL
[0085] Weigh 10 mg of compound I hydrochloride sample of an experimental batch in a 50 mL volumetric flask, add 1 mL of methanol to dissolve the sample completely, then add mobile phase to dilute the sample to the scale, and make a test solution with a concentration of about 0.2 mg / mL , according to the above-mentioned chromatographic conditions, the test solution is analyzed to obtain the following Figure 4 The liquid chromatogram shown. The retention time of compound Ⅰ was 6.40 min, and the retention time of its enantiomer compound Ⅱ was 5.01 min. The content of compound Ⅱ was 0.9% by area normalization method, and the ee% of compound Ⅰ was 98.2%.
Embodiment 3
[0087] Chromatographic conditions
[0088] Mobile phase: V 正己烷 :V 乙醇 :V 甲醇 =90:9:1;
[0089] Flow rate: 1.0mL / min;
[0090] Detection wavelength: 220nm;
[0091] Column temperature: 25°C;
[0092] Injection volume: 20μL
[0093] Weigh 10 mg of compound I hydrochloride sample of an experimental batch in a 50 mL volumetric flask, add 1 mL of methanol to dissolve the sample completely, then add mobile phase to dilute the sample to the scale, and make a test solution with a concentration of about 0.2 mg / mL , according to the above-mentioned chromatographic conditions, the test solution is analyzed to obtain the following Figure 5 The liquid chromatogram shown. The retention time of compound Ⅰ was 7.81 min, and the retention time of its enantiomer compound Ⅱ was 5.93 min. The content of compound Ⅱ was 0.7% by area normalization method, and the ee% of compound Ⅰ was 98.6%.
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