Lactam histone deacetylase inhibitors
A technology of benzamide and compound, applied in the field of medicinal chemistry
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Embodiment 1
[0090] (E)-N-(2-Aminophenyl)-4-((2-oxo-3-(pyridin-2-ylmethylene)piperidin-1-yl)methyl)benzamide
[0091]
[0092] Step a: Preparation of tert-butyl-2-oxopiperidine-1-carboxylic acid
[0093] Add piperidin-2-one (5g, 50mmol), di-tert-butyl dicarbonate (13.1g, 60mmol), and acetonitrile 100mL in a 250mL eggplant-shaped flask. Cool to 0℃ in an ice bath, and slowly add 4-dicarbonate in batches. Methylaminopyridine (1.22g, 10mmol, after addition, react at room temperature for 24h, TLC detects that the reaction is complete, the solvent is evaporated under reduced pressure, the residue is separated by silica gel column chromatography (petroleum ether: ethyl acetate = 15:1) Color oily liquid (6.07g, 30.5mmol). 1 H-NMR(300MHz, CDCl 3 )δ3.65(m, 2H), 2.50(m, 2H), 1.82(m, 4H), 1.52(s, 9H). ESIMS: [M+H] + : 222.12.
[0094] Step b: (E)-tert-Butyl-2-oxo-3-(pyridin-2-ylmethylene)piperidine-1-carboxylic acid tert-butyl ester
[0095] Add tert-butyl-2-oxopiperidine-1-carboxylic acid (4g, 20mmol) in a ...
Embodiment 2
[0105] (E)-N-(2-Amino-4-fluorophenyl)-4-[[2-oxo-3-(pyridin-2-ylmethylene)piperidin-1-yl]methyl]benzene Formamide
[0106]
[0107] Using piperidin-2-one, 4-fluoro-1,2-phenylenediamine as raw materials, pyridine-2-carboxaldehyde, and methyl p-bromomethyl benzoate, the target compound white was prepared by a method similar to Example 1 Solid (E)-N-(2-amino-4-fluorophenyl)-4-[[2-oxo-3-(pyridin-2-ylmethylene)piperidin-1-yl]methyl] Benzamide, the yield is 41.1%; Mp: 217-219°C; 1 H-NMR (300MHz, DMSO-d6) δ 9.60 (s, 1H), 8.67 (d, J = 3.9 Hz, 1H), 7.96 (d, J = 8 Hz, 1H), 7.87-7.81 (m, 1H) , 7.63 (s, 1H), 7.55 (d, J = 7.9 Hz, 1H), 7.40 (d, J = 8.1 Hz, 2H), 7.34-7.30 (m, 1H), 7.13-7.08 (m, 1H), 6.53(dd, J=11.3, 3Hz, 1H), 6.39-6.32(m, 1H), 5.25(s, 2H), 4.73(s, 2H), 3.4(s, 2H), 3.18-3.15(m, 2H) ), 1.82-1.80(m, 2H).ESIMS: [M+Na] + : 453.2.
Embodiment 3
[0109] (E)-N-(2-Aminophenyl-4-[[3-(furan-2-ylmethylene)-2-oxopiperidin-1-yl]methyl]benzamide
[0110]
[0111] The preparation method is as in Example 1, and a white solid is obtained with a yield of 62.3%. Mp: 212-214°C; 1 H-NMR(300MHz, DMSO-d 6 )δ9.66(s, 1H, -CONHAr-), 7.95(d, J=8Hz, 2H, H-Ar), 7.84(d, J=8Hz, 2H, H-Ar), 7.84-7.83(m, 1H, H-Ar), 7.62 (s, 1H, -CH=), 7.4 (d, J=1 Hz, 2H, H-Ar), 7.12-7.08 (m, 1H, H-Ar), 6.80 (d, J=3.3Hz, 1H, H-Ar), 6.66-6.64 (m, 1H, H-Ar), 6.53 (dd, J 1 =11Hz, J 2 = 3Hz, 1H, H-Ar), 6.39-6.32 (s, 1H, H-Ar), 5.24 (s, 2H, -NH 2 ), 4.65(s, 2H, -CH 2 -), 2.88(s, 2H, -CH 2 -), 1.84(s, 2H, -CH 2 -), 1.24(m, 2H, -CH 2 -); IR(KBr cm -1 ): 3457, 3348, 3292, 3104, 2989, 2949, 2389, 1728; MS m / z: 424.2 [M+Na] + .
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