1-Chloro-3,5-Di-(4-Chlorobenzoyl)-2-Deoxy-D-Ribose CAS 3601-90-9; 21740-23-8 Assay >90.0% (HPLC) Trifluridine Decitabine Intermediate

1-Chloro-3,5-Di-(4-Chlorobenzoyl)-2-Deoxy-D-Ribose (CAS: 21740-23-8) Method of Analysis
Properties: This product is white or off-white powder.
Identification: The infrared spectrum of this product should be consistent with that of the reference product (Appendix IV C of the second part of the 2010 edition of Chinese Pharmacopoeia).
Analysis: Related substances. Take an appropriate amount of this product, weigh it accurately, dissolve it with acetonitrile-water (80:20) and dilute it quantitatively to make a solution containing about 0.5mg in every 1ml as the test product solution. According to the chromatographic conditions under the content determination item, the sample solution of 10μl was precisely measured, injected into the high performance liquid chromatograph (HPLC) equipment, and the chromatogram was recorded. If there is an impurity peak in the solution chromatogram of the test product, the impurity 1 (relative retention time is about 0.14) shall not exceed 2.5%, impurity 2 (relative retention time is about 2.1) shall not exceed 5.0%, impurity 3 (relative retention time is about 2.3) shall not exceed 1.5%, and other single impurity shall not exceed 0.5%, according to the area normalization method. Total impurities must not exceed 10.0%
Loss on drying: Take an appropriate amount of this product, phosphorus pentoxide as a desiccant, drying at 40℃ vacuum to constant weight, weight loss should not exceed 1.0% (Chinese Pharmacopoeia 2010 edition, Part II Appendix Ⅷ L).
Assay: According to high performance liquid chromatography (Chinese Pharmacopoeia 2010, Part II Appendix V D) determination.
Chromatographic conditions and system suitability test: Octadecylsilane bonded silica gel was used as filler (specification: 4.6×250mm, 5μm), 0.01mol/L potassium dihydrogen phosphate solution (pH adjusted to 6.5 by 1mol/L potassium hydroxide solution) -acetonitrile (90:10) as mobile phase A, acetonitrile as mobile phase B, and linear gradient elution was performed according to the following table. The detection wavelength was 205nm; The column temperature was 30℃, the flow rate was 1ml per minute, and the sample chamber temperature was 2~8℃. The separation degree between the main peak and adjacent impurity peaks should meet the requirements.
Time (min) Mobile phase A (%) Mobile phase B (%)
0 50 50
20 50 50
40 33 67
55 33 67
56 50 50
65 50 50
Measurement: Take an appropriate amount of this product, weigh it accurately, dissolve it with acetonitrile-water (80:20) and dilute it quantitatively to make a solution containing about 0.5mg in every 1ml as the test product solution. The sample solution of 10μl was accurately measured, injected into the high performance liquid chromatograph (HPLC) equipment, and the chromatogram was recorded. According to the area normalization method, the main peak content should not be less than 90.0%.
Storage: Dark, sealed, stored in a cold place.
Validity: 12 months.