Imidazol[4,5-b]pyridine thioethanamide derivatives, preparation method and application thereof
A technology of azole thioacetamide and derivatives, which can be used in drug combinations, pharmaceutical formulations, and medical preparations containing active ingredients, etc., can solve the problems of easy mutation of amino acid residues, spread of drug-resistant strains, and clinical application limitations.
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Embodiment 1
[0038] Example 1: Methyl 3-bromo-4-(2-(1(4-cyclopropylnaphthalen-1-yl)-1 hydrogen-imidazo[4,5-b]pyridine-2-mercapto)acetamido ) preparation of benzamide (I-1)
[0039] Trifluoromethanesulfonic anhydride (0.35g, 0.142mmol) was slowly added dropwise to a dichloromethane solution of 2-nitro-hydroxypyridine (0.1g, 0.71mmol) and triethylamine (0.11g, 1.065mmol) under stirring in an ice bath Medium (10 mL). After the reaction solution was stirred for three hours, 50 mL of water was added, extracted with dichloromethane (2×10 mL), the organic layer was combined with saturated brine, washed twice, dried over anhydrous sodium sulfate, filtered and concentrated to obtain intermediate 2. Purple-black oil, yield: 94.9%. ESI-MS: m / z 271.3 (M-1), C 6 h 3 f 3 N 2 o 5 S[271.97].
[0040] 4-Bromo-1-naphthylamine (3) (0.50g, 2.25mmol), cyclopropyl boronic acid (0.212g, 2.47mmol), tetrakistriphenylphosphine palladium (0.26g, 0.23mmol), potassium phosphate (1.67g , 7.87mmol) were weighed...
Embodiment 2
[0045] Example 2: Methyl 3-bromo-4-(2-(1-(4-cyclopropylnaphthalen-1-yl)-1 hydrogen-imidazo[4,5-b]pyridine-2-mercapto)acetamide Base) the preparation of benzamide (I-2)
[0046] The operation method is the same as that of Example 1 (I-1), except that methyl 3-bromo-4-(2-chloroacetamido)benzamide is used. White powder, yield: 45.2%.mp: 135-137℃. 1 H NMR (400MHz, DMSO-d 6 ,ppm)δ:10.16(s,1H,NH),8.62(d,1H,J=8.0Hz,pyridylimidazole-H),8.43(d,1H,J=4.0Hz,naphthaline-H),8.13(s, 1H, PhH), 8.08 (d, 1H, J = 8.0Hz, pyridylimidazole-H), 7.95 (d, 1H, J = 8.0Hz, naphthaline-H), 7.72 (d, 2H, J = 8.0Hz, naphthaline- H), 7.53 (t, 1H, J = 8.0Hz, pyridylimidazole-H), 7.49 (d, 1H, J = 8.0Hz, PhH), 7.31 (d, 2H, J = 8.0Hz, naphthaline-H), 7.17 (dd,2H,J 1 =8.0Hz,J 2 =4.0Hz,naphthaline-H),7.12(d,1H,J=8.0Hz,PhH),4.47(m,2H,S-CH 2 ),4.33(q,2H,J=4Hz,CH 2 ), 2.61-2.56(m, 1H, cyclopropyl-H), 1.33(t, 3H, J=4.0Hz, CH 3 ),1.19-1.16(m,2H,cyclopropyl-H),0.91-0.87(m,2H,cyclopropyl-H). 13 C-NMR (100MHz, DM...
Embodiment 3
[0047] Example 3: N-(2-bromo-4 cyanophenyl)-2-(1-(4-cyclopropylnaphthalen-1-yl)-1 hydrogen-imidazo[4,5-b]pyridine-2 -The preparation of mercapto) acetamide (I-3)
[0048] The operation method is the same as that of Example 1 (I-1), except that N-(2-bromo-4cyanophenyl)-2-chloroacetamide is used. White powder, yield: 41.3%.mp: 214-215℃. 1 H NMR (400MHz, DMSO-d 6 ,ppm)δ:10.25(s,1H,NH),8.62(d,1H,J=8.00Hz,pyridylimidazole-H),8.43(d,1H,J=4.0Hz,naphthaline-H),8.25(d, 1H, J = 4.0Hz, PhH), 8.11 (d, 1H, J = 8.0Hz, pyridylimidazole-H), 7.87 (d, 1H, J = 8.0Hz, naphthaline-H), 7.74-7.70 (m, 2H, naphthaline-H), 7.55 (t, 1H, J = 8.0Hz, pyridylimidazole-H), 7.48 (d, 1H, J = 8.0Hz, PhH), 7.31 (dd, 1H, J 1 =8.0Hz,J 2 =4.0Hz,naphthaline-H),7.17(dd,1H,J 1 =8.0Hz,J 2 =4.0Hz,naphthaline-H),7.11(d,1H,J=8.0Hz,PhH),4.49-4.39(m,2H,S-CH 2 ),2.62-2.55(m,1H,cyclopropyl-H),1.19-1.15(m,2H,cyclopropyl-H),0.91-0.87(m,2H,cyclopropyl-H). 13 C-NMR (100MHz, DMSO-d 6 ,ppm)δ:167.41(C=O),156.86,155.62,144....
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