A class of compounds that improve the sensitivity of pca drug-resistant cells to antagonists and their use
A technology of drug-resistant cells and compounds, applied in the field of medicine, can solve problems such as hot flashes in patients, and achieve the effect of improving sensitivity
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Embodiment 1
[0051] Embodiment 1, the synthesis of compound JT-21
[0052] The synthetic route of compound JT-21 is shown in the following formula:
[0053]
[0054] Experimental procedures and results of compound JT-21:
[0055] Step 1: Synthesis 2
[0056]
[0057] Compound 1 (2.24g, 10mmol, 1.0eq) was added into absolute ethanol (30mL), then 4-isopropylaniline (2.03g, 15mmol, 1.5eq) was added to the above solution, and reacted at 75°C for 20h. The reaction solution was cooled to room temperature, and the precipitated solid was filtered, washed with a small amount of ethanol and dried to obtain the target product (1.8 g, 51%, white solid).
[0058] 1 HNMR (400MHz, CDCl3): δ8.39(s, 1H), 7.60(d, J=8.4Hz, 2H), 7.27(d, J=8.6Hz, 2H), 7.19(br s, 1H), 4.37( q, J=7.1Hz, 2H), 3.04–2.86(m, 1H), 2.83(s, 3H), 1.42(t, J=7.1Hz, 3H), 1.29(d, J=6.9Hz, 6H).
[0059] LCMS: (M+H)+: 324.2.
[0060] Step 2: Synthesis 3
[0061]
[0062] Compound 2 (0.5g, 1.55mmol, 1.0eq) was dissolved in et...
Embodiment 2
[0071] Embodiment 2, the synthesis of compound JT-22
[0072] The synthetic route of compound JT-22 is shown in the following formula:
[0073]
[0074] Experimental procedures and results of compound JT-22:
[0075] Compound JT-21 (65mg, 0.2mmol, 1.0eq) was dissolved in methanol (2mL) and tetrahydrofuran (2mL), then lithium hydroxide (25mg, 0.6mmol, 3eq) aqueous solution (2mL) was added dropwise to the above solution, React overnight at room temperature. The organic phase was spin-off, the aqueous phase was extracted with ethyl acetate (2x5mL), then the pH of the aqueous phase was adjusted to 3 with 2N dilute hydrochloric acid, the precipitated solid was filtered, washed with a small amount of water and dried to obtain the target product (40mg, 67 %, white solid).
[0076] 1 HNMR(400MHz,DMSO-d6):δ13.14(br s,1H),12.43(s,1H),8.98(s,1H),8.04(d,J=1.8Hz,1H),7.72(dd,J =8.6,1.9Hz,1H),7.60(d,J=8.6Hz,1H),3.09–2.97(m,1H),2.85(s,3H),1.27(d,J=6.9Hz,6H).
[0077] LCMS: (M+H)+: ...
Embodiment 3
[0079] Embodiment 3, the synthesis of compound JT-38
[0080] The synthetic route of compound JT-38 is shown in the following formula:
[0081]
[0082] Experimental procedures and results of compound JT-38:
[0083] Step 1: Synthesis 2
[0084]
[0085]Compound 1 (300mg, 1mmol, 1eq) was dissolved in ethanol (10mL), concentrated sulfuric acid (1mL) was added thereto, and the reaction was refluxed for 60 hours. The reaction solution was cooled to room temperature, filtered, and the filter cake was washed with a small amount of ethanol, collected and dried to obtain the target compound 2 (300 mg, crude product, off-white solid).
[0086] 1 HNMR (400MHz, DMSO-d6): δ8.81(s, 1H), 8.37(br s, 1H), 8.11(br s, 1H), 7.93(d, J=1.9Hz, 1H), 7.75(dd, J=8.6,2.1Hz,1H),7.55(d,J=8.6Hz,1H),4.36(q,J=7.2,2H),3.13–2.99(m,1H),1.37(t,J=7.1Hz ,3H),1.26(d,J=6.9Hz,6H).
[0087] LCMS: (M+H)+: 327.1.
[0088] Step 2: Synthesis of JT-38
[0089]
[0090] Compound 2 (100mg, 0.31mmol, 1.0e...
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