Preparation and detection method of azo compound
A compound, sodium iodide technology, used in measuring devices, instruments, scientific instruments, etc., can solve problems such as hazards and hidden dangers in drug safety
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[0092] Preparation of Compound C:
[0093]
[0094] Method 1: Add compound A (12.47g, 1.0eq) and methanol (125mL, 10V) to a 250mL double-neck flask at room temperature, stir and then add NH 4 The solution prepared by Cl (3.1g, 1.5eq) and water (60mL, 5V) and zinc powder (7.58g, 3.0eq) were vacuum-replaced with nitrogen three times and then heated to 65°C, reacted for 5h, and HPLC monitored that compound A was less than 5.0 %, the reaction was completed, cooled to room temperature, filtered, and the filtrate was transferred to a 250 mL single-neck bottle; the temperature was raised to 50 ° C and stirred for 10 h, and then sampled. (50mL) beating for 1h, suction filtration, the wet product is dried under vacuum (-0.09Mpa) at 60°C for 16h to obtain compound C: 6.27g, purity 96.65%, yield 54.3%; Detection: ESI-MS (m / z ):525.3(M+H+); 1 H NMR (400MHz, DMSO-d 6 )δ9.18(brs,4H),8.22(d,J=8.0Hz,2H),8.10(d,J=8.0Hz,2H),7.53(d,J=8.0Hz,2H),7.42(m, 8H), 7.33 (m, 2H), 6.28 (d, 2H), 5.15...
Embodiment 1
[0097]
[0098] Compound C (3 g), 10% Pd / C (0.15 g) and methanol (60 mL) were added to a 100 mL double-necked bottle, and the hydrogen was vacuum-replaced three times. HPLC detected that the content of compound C was less than 1.0%, the reaction was completed, suction filtration, and the filtrate was rotary evaporated to a solid to obtain compound D: 2.7 g, the purity was 96.32%, and the yield was 92.2%; ESI-MS (m / z) : 511.3 (M+H+).
[0099]
[0100] Compound D (1.0g, 1.0eq), sodium iodide (0.59g, 2.0eq) and acetonitrile (30mL) were added to a 50mL double-necked flask, nitrogen was vacuum replaced three times, and t-BuOCl (0.43g, 2.0eq) was added with a syringe ), stirred and reacted at room temperature (25°C) for 6 h and sampled for inspection. HPLC detected that the reaction compound D was less than 1.0%. After the reaction was completed, suction filtration was performed, rinsed with acetonitrile (3 mL) and dried, and the wet product (1.05 g) was added to methanol (10 ...
Embodiment 2
[0102] Instruments and Conditions
[0103]
[0104] Experimental procedure
[0105] Mobile phase Phase A: namely 0.1% formic acid aqueous solution, add 1 mL of formic acid to 1000 mL of ultrapure water, mix well, and sonicate for 10 minutes;
[0106] Mobile phase B phase: acetonitrile;
[0107] Diluent / blank solution: methanol;
[0108] Reference substance stock solution 1: Precisely weigh 37.5 mg of each of compound C and compound E into a 100 mL volumetric flask, add an appropriate amount of methanol to dissolve by ultrasonic, and then dilute to the mark to obtain;
[0109] Reference substance stock solution 2: Precisely pipette 1mL of reference substance stock solution 1 to 50mL volumetric flask, dilute to volume with methanol, and shake well;
[0110] Reference substance stock solution 3: Precisely pipette 1mL of reference substance stock solution 2 to 10mL volumetric flask, dilute to volume with methanol, and shake well;
[0111] Reference substance solution: Preci...
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