Amide compounds with antitumor activity and application of amide compounds
An amide compound, anti-tumor activity technology, applied in the field of medicine, to achieve good inhibitory effect
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Embodiment 1
[0044] Example 1: Synthesis of Compound (1)
[0045]
[0046] Dissolve 1.6 g of 4-aminophenoxycarbonyl chloride, 7.98 mmol, 1.05 N (N represents the molar ratio) in 8 mL of dichloromethane, and then add 3,4-dichloromethane dropwise at 0°C under nitrogen protection. Methylaniline 970mg, 8.00mmol, 1.05N was dissolved in 12mL of dichloromethane mixed solution, continued stirring for 2h after the dropwise addition, and then added N-ethyl-N isopropylpropyl-2-amine 1.47g, 11.38g mmol, 1.50N and 2-nitro-5-(piperidinyl-1) phenylhydrazine 2.0g, 7.26mmol, 1.00N, 96%, stir for 3h, add dichloromethane 150mL to dilute, use 200mL saturated sodium chloride It was dissolved in water and washed 3 times, dried over anhydrous sodium sulfate, concentrated under reduced pressure, and finally separated and purified by silica gel column chromatography. Yellow solid 4-(3,4-dimethylphenyl)-1-(2-nitro-5-(piperidinyl-1)benzoyl) semi-bisemicarbazide 2.0 g, yield 67%, ( ES,m / z):412.2[M+H] +1 .
[0...
Embodiment 2
[0050] Example 2: Synthesis of Compound (2)
[0051]
[0052] Dissolve benzoyl isothiocyanate 1.5g, 9.09mmol, 1.00N in acetone 15mL, then add 3-(trifluoromethyl)aniline 1.5g, 9.32mmol, 1.02N, the whole system was stirred at 0 °C overnight , concentrated under reduced pressure to obtain off-white solid 1-benzoyl-3-(3-(trifluoromethyl)phenyl)thiourea 2.7g, yield 92%, (ES, m / z): 325.2[M+ H] +1 , 327.2[M+H+2] +1 .
[0053] The above-mentioned off-white solid 3.2g, 9.88mmol, 1.00N was dissolved in 50mL methanol, then sodium hydroxide 565mg, 14.12mmol, 1.43N, purified water 40mL was added, and the whole system was stirred at 80°C for 2h and concentrated under reduced pressure. Extracted with 30 mL×3 of methane, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to obtain 2 g of 1-(3-(trifluoromethyl)phenyl)thiourea as a light yellow solid, yield 92%, (ES, m / z) :221.2[M+H] +1 , 223.2[M+H+2] +1 .
[0054] The above-mentioned light yellow solid 1g, 4...
Embodiment 3
[0058] Example 3: Synthesis of Compound (3)
[0059] The difference from Example 1 is that 2-nitro-5-(piperidine-1)-thio-benzylmethylhydrazine is used as a raw material, and compound (3) can be obtained according to the synthetic method of Example 1. ), the specific structural formula is as follows:
[0060]
[0061] (ES,m / z):635.2[M+H] +1 , 637.2[M+H+2] +1 ;HNMR(300MHz, CDCl 3 )δ:9.05-9.02(d,J=9.3Hz,1H),8.45(s,1H),8.24-8.13(m,2H),8.10-7.87(m,2H),7.84-7.70(m,1H) ,7.51-7.45(m,3H),7.29-7.26(d,J=7.8Hz,1H),3.98-3.95(s,2H),3.72-3.64(m,4H),3.45-3.41(m,2H) ,3.26-3.19(m,5H),3.12-3.08(m,2H),2.52(s,3H),2.08-2.06(m,4H),1.86-1.85(m,2H),1.37-1.29(m, 6H). See image 3 .
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