Compound with sulfonyl phenylamine pyrimidine structure and application of compound as antitumor medicine
A technology containing sulfonanilidine and sulfonanilidine, which is applied in the application field of treating malignant tumors and diseases related to differentiation and proliferation, can solve the problems of weak EGFR kinase inhibitory activity and decreased tumor growth rate, and achieves a good choice Inhibitory activity, anti-tumor clinical application prospect, effect of good clinical application prospect
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Embodiment 1
[0073] N-(3-fluoro-4-((2-((3-sulfonamido)amino)pyrimidine)-4-oxyl)phenyl)-N-(4-fluorophenyl)cyclopropyl-1, Preparation of 1-dicarboxamide (I-1) and its salt
[0074] Prepare according to the synthetic general method, and the specific operation is as follows:
[0075] Preparation of intermediate 1-((4-fluorophenyl)carbamoyl)cyclopropanecarboxylic acid (1-1):
[0076] Dissolve cyclopropane-1,1-dicarboxylic acid (13.01g, 0.10mol) in THF 120mL, under nitrogen protection, slowly add triethylamine (10.12g, 0.10mol) dropwise at 0°C, stir for 15min, then slowly Add SOCl dropwise 2(9.95g, 0.10mol), maintain this temperature and continue to stir for 30min. 60 mL of THF solution dissolved in 4-fluoroaniline (12.22 g, 0.11 mol) was added dropwise, and the reaction was completed under ice bath conditions. The reaction solution was adjusted to pH 9.0 with 10% sodium hydroxide solution, and after stirring for 10 min, the pH was adjusted to 5.0 with 1N HCl to precipitate a solid, which wa...
Embodiment 2
[0092] N-(4-fluorophenyl)-N-(4-((2-((3-sulfonamidophenyl)amino)pyrimidine)-4-oxyl)phenyl)cyclopropyl-1,1- Preparation of Diformamide (I-2) and Its Salts
[0093] According to the general synthesis method, the target compound I-2 was prepared with a yield of 56%, ESI-MS (m / z): 563.15[M+H]+. 1 H NMR (400Hz, DMSO-d 6 )δppm: 10.31(s,1H,NH),10.12(s,1H,NH),9.90(s,1H,NH),8.42(d,1H,J=4.0Hz,ArH),8.04(s,1H, ArH),7.81(m,1H,ArH),7.73(d,1H,J=8.0Hz,ArH),7.65(m,4H,ArH),7.30(m,5H,ArH),7.16(m,2H, NH 2 ), 6.60(d, 1H, J=8.0Hz, ArH), 1.47(d, 4H, J=8.0Hz, CH 2 ).
[0094] The preparation of compound 1-2 hydrobromide:
[0095] Using compound I-2 (2.0 mmol) and 5% hydrobromic acid aqueous solution (2.1 mmol) as raw materials, the preparation method of compound I-1 hydrobromide was used to obtain 0.9 g of white I-2 hydrobromide as a solid.
Embodiment 3
[0097] N-(3-fluoro-4-((2-((3-(methylsulfonamido)phenyl)amino)pyrimidine)-4-oxyl)phenyl)-N-(4-fluorophenyl) Preparation of cyclopropyl-1,1-dicarboxamide (I-3) and its salt
[0098] According to the general method of synthesis, the target compound I-3 was prepared with a yield of 43%, ESI-MS (m / z): 595.11
[0099] [M+H] + . 1 H NMR (400Hz, DMSO-d 6 )δppm: 10.36(s,1H,NH),10.05(s,1H,NH),9.93(s,1H,NH),8.42(d,1H,J=4.0Hz,ArH),8.04(s,1H, ArH),7.81(m,1H,ArH),7.73(d,1H,J=8.0Hz,ArH),7.65(m,2H,ArH),7.46(d,1H,J=8.0Hz,ArH),7.30 (m,5H,ArH),7.11(m,1H,NH),6.60(d,1H,J=8.0Hz,ArH),2.93(s,3H,CH 3 ), 1.41 (d, 4H, J=8.0Hz, CH 2 ).
[0100] The preparation of compound 1-3 malate:
[0101] Compound I-1 (0.1 mmol) and malic acid (0.8 mmol) were added to ethanol (10 mL), dissolved under reflux, and a white solid was precipitated by cooling, and filtered to obtain 0.12 g of white I-3 malate solid.
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