Bis-aryl amine compound as well as preparation method and application thereof
A compound and aromatic-based technology, which is applied in the field of bis-arylamine compounds and their preparation, can solve problems such as hindering the use of anti-androgen drugs
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Embodiment 1
[0087] The preparation of embodiment 1 compound 1
[0088] Under anhydrous conditions, 3-(1H-pyrazol-5-yl)aniline (100.0 mg, 0.63 mmol) was dissolved in anhydrous DMF (5.0 mL), and anhydrous K 2 CO 3 (130.2mg, 0.94mmol), under ice-water bath conditions (0°C), add 4-acetylbenzenesulfonyl chloride (164.8mg, 0.75mmol) to the solution, react at 0-4°C for 30min, then turn to room temperature reaction, After 6-8h, TLC showed that 3-(1H-pyrazol-5-yl)aniline disappeared, and the reaction was stopped. The reaction solution was diluted with ethyl acetate, the aqueous phase was tested with PH test paper, and NaHCO 3 Adjust the pH of the saturated solution between 9-11, wash with water, wash with saturated NaCl solution, anhydrous NaCl 2 SO 4 Drying, concentration, separation and purification by column chromatography (PE / EA=1.5 / 1V / V) gave white floc 1 (112.4 mg, yield: 52.3%).
[0089] Compound 1 was detected by H NMR spectrum ( 1 HNMR) and high resolution mass spectrometry (HRMS) a...
Embodiment 2
[0092] The preparation of embodiment 2 compound 2
[0093] Under anhydrous conditions, 3-(1H-pyrazol-5-yl)aniline (100.0 mg, 0.63 mmol) was dissolved in anhydrous DMF (5.0 mL), and anhydrous K 2 CO 3 (130.2mg, 0.94mmol), under ice-water bath conditions (0°C), 4-fluorobenzenesulfonyl chloride (146.9mg, 0.75mmol) was added to the solution, reacted at 0-4°C for 30min, then turned to room temperature reaction, 6 -8h later, TLC showed that 3-(1H-pyrazol-5-yl)aniline disappeared, and the reaction was stopped. The reaction solution was diluted with ethyl acetate, the aqueous phase was tested with PH test paper, and NaHCO 3 Adjust the pH of the saturated solution between 9-11, wash with water, wash with saturated NaCl solution, anhydrous NaCl 2 SO 4 Drying, concentration, separation and purification by column chromatography (PE / EA=1.5 / 1V / V) gave white floc 2 (140.3 mg, yield: 70.2%).
[0094] Compound 2 was detected by H NMR spectrum ( 1 HNMR) and high resolution mass spectromet...
Embodiment 3
[0097] The preparation of embodiment 3 compound 3
[0098] Under anhydrous conditions, 3-(1H-pyrazol-5-yl)aniline (100.0 mg, 0.63 mmol) was dissolved in anhydrous DMF (5.0 mL), and anhydrous K 2 CO 3 (130.2mg, 0.94mmol), under ice-water bath conditions (0°C), add 4-chlorobenzenesulfonyl chloride (159.3mg, 0.75mmol) to the solution, react at 0-4°C for 30min, then turn to room temperature reaction, 6 -8h later, TLC showed that 3-(1H-pyrazol-5-yl)aniline disappeared, and the reaction was stopped. The reaction solution was diluted with ethyl acetate, the aqueous phase was tested with PH test paper, and NaHCO 3 Adjust the pH of the saturated solution between 9-11, wash with water, wash with saturated NaCl solution, anhydrous NaCl 2 SO 4 Drying, concentration, separation and purification by column chromatography (PE / EA=1.5 / 1V / V) gave white floc 3 (118.5 mg, yield: 56.4%).
[0099] Compound 3 was detected by H NMR spectrum ( 1 HNMR) and high resolution mass spectrometry (HRMS) ...
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