Piperidone derivatives with antitumor activity and preparation method thereof
A technology of anti-tumor activity and piperidone, which is applied in the direction of anti-tumor drugs, drug combinations, organic chemistry, etc., can solve the problems of unstable chemical structure, low bioavailability, poor water solubility, etc., to avoid genotoxicity, preparation method Simplicity and high synthesis yield
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Embodiment 1
[0020] Synthesis of N-methyl-3,5-bis(3-aminobenzylidene)-4-piperidone
[0021] Mix 0.01mol of N-methyl-4-piperidone and 0.022mol of m-nitrobenzaldehyde in a solution of 20mL of methanol and water, add 20mL of 20% sodium hydroxide solution at room temperature, stir and react at room temperature for 12h, pass through a thin Thin layer chromatography (TLC) analysis confirmed the reaction end point. The precipitate was suction filtered to obtain the intermediate as light yellow powder. Add the intermediate and 0.065mol of stannous chloride to 25mL of concentrated hydrochloric acid and stir for 6-8h, and determine the end point of the reaction through thin-layer chromatography (TLC) analysis, precipitate and suction filter, 10% sodium carbonate solution lotion, 15mL ethanol / Water (volume ratio 1:1) was recrystallized to obtain a yellow powder, namely N-methyl-3,5-bis(3-aminobenzylidene)-4-piperidone.
Embodiment 2
[0023] N-methyl-3,5-bis(3-(2,3-dihydroxybenzylideneamino)benzylidene)-4-piperidone (A)
[0024] Dissolve 0.001mol of N-methyl-3,5-bis(3-aminobenzylidene)-4-piperidone and 0.003mol of 2,3-dihydroxybenzaldehyde in 40mL of methanol, add 3 drops of formic acid dropwise, and The reaction was stirred for 8 h, and the end point of the reaction was determined by thin layer chromatography (TLC) analysis. The precipitate was suction filtered, washed with methanol, and dried under vacuum to obtain red powder N-methyl-3,5-bis(3-(2,3-dihydroxybenzylideneamino)benzylidene)-4-piperidone (A) 0.3133 g, yield 56%.
[0025] IR (cm -1 ):3253(br),1614(s),1573(s),1460(m),1363(m),1273(s),1209(s),1183(m),1028(w),939(w ),850(w),789(m),734(s),684(s),540(w). 1 HNMR(400MHz,DMSO,25℃,TMS,ppm):δ13.03(s,2H),9.26(s,2H),8.97(s,2H),7.69(s,2H),7.62-7.50(m, 4H), 7.50-7.40(m, 4H), 7.13(d, J=8Hz, 2H), 6.98(d, J=8Hz, 2H), 6.81(t, J=8Hz, 2H), 3.82(s, 4H ),2.42(s,3H).13CNMR(100MHz,CDCl 3 ):186.27,164.75,149.25,...
Embodiment 3
[0027] N-methyl-3,5-bis(3-(2,4-dihydroxybenzylideneamino)benzylidene)-4-piperidone (B)
[0028] Dissolve 0.001mol of N-methyl-3,5-bis(3-aminobenzylidene)-4-piperidone and 0.0035mol of 2,4-dihydroxybenzaldehyde in 45mL of methanol, add 6 drops of formic acid dropwise, and The reaction was stirred for 9 h, and the end point of the reaction was determined by thin layer chromatography (TLC) analysis. The precipitate was suction filtered, washed with methanol, and dried in vacuo to obtain yellow powder N-methyl-3,5-bis(3-(2,4-dihydroxybenzylideneamino)benzylidene)-4-piperidone (B) 0.3025 g, yield 54%.
[0029] IR (cm -1 ):3144(br),1672(w),1607(s),1568(s),1509(w),1455(w),1329(w),1281(w),1208(s),1176(m ),1127(m),977(m),850(m),788(s),691(s),651(w),538(w). 1 HNMR (400MHz, DMSO, 25℃, TMS, ppm): δ13.38(s, 2H), 10.50(s, 2H), 8.84(s, 2H), 7.66(s, 2H), 7.53(t, J= 8Hz, 2H), 7.46(d, J=8Hz, 4H), 7.38(t, J=8Hz, 4H), 6.43(d, J=8Hz, 2H), 6.31(s, 2H), 3.78(s, 4H ),2.40(s,3H). 13 CNMR (100MH...
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