4-Amino-5-Chloro-2,3-Dihydrobenzofuran-7-Carboxylic Acid CAS 123654-26-2 Prucalopride Succinate Intermediate Purity ≥98.0% (HPLC)

This product is 4-Amino-5-Chloro-2,3-Dihydrobenzofuran-7-Carboxylic Acid, the content of C12H12ClNO4 shall not be less than 98.0%, calculated on the anhydrous basis.
[Properties] This product is off-white to light-red solid.
[Check]
Take an appropriate amount of this product (about 0.5g) of water, add solvent (methanol: N,N-dimethylformamide = 50:50), and dissolve it according to water determination method (Appendix Ⅷ M, first method A). Use Fisher's test drops to determine until the solution changes from light yellow to reddish-brown indicating end point, and conduct another blank test. Calculate according to the following formula: the water content should not exceed 1.00%.
Moisture content (%) = (A-B) F/W×100%
Where, A is the volume of Fisher's liquid consumed by the test product (ml);
B is the volume of Fisher's test liquid consumed by blank space, ml;
F is the weight of Fisher's test solution equivalent to water per 1ml, mg;
W is the weight of the test product, mg
Related substance
According to the method under "Content measurement item", if there are impurity peaks in the chromatogram of the test solution, the peak area of a single impurity shall not be greater than 10 times (1.0%) of the main peak area of the control solution, and the sum of the peak area of all impurities shall not be greater than 20 times (2.0%) of the main peak area of the control solution.
[Content Determination] According to high performance liquid chromatography (Appendix VI D).
Octadecylsilane bonded silica gel was used as filler for chromatographic conditions and system suitability tests. Phosphate buffer solution (1.36g potassium dihydrogen phosphate, dissolved ultrasonic in 1L water, phosphoric acid adjusted to PH 3.0) was used as mobile phase A. Acetonitrile is mobile phase B, and gradient elution is performed according to the following table:
Time (min) Mobile phase A mobile phase B
0 80 20
15 80 20
30 50 50
45 50 50
The detection wavelength was 254 nm. The flow rate was 1.0 ml/min. The number of theoretical plates is not less than 2000 according to the peak of 4-Amino-5-Chloro-2,3-Dihydrobenzofuran-7-Carboxylic Acid
The peak of furanoformic acid is not less than 2000.
Determination method:
Take 10mg of the test product, weigh it accurately, put it in A 10ml bottle, dissolve it ultrasonic with mobile phase A-mobile phase B (70:30) as the solvent, dilute it to the scale, shake well, and prepare a solution with a concentration of 1mg/ml. 20 l of precision was injected into the liquid chromatograph, and the chromatogram was recorded. The main peak purity was not less than 98.0% according to the peak area normalization method
Column: Dionex Acclaim C18, 4.6*250mm, 5um
Column temperature: 40℃
Flow rate: 1.0ml/min
Detection wavelength: 254nm
Sample size: 10μL