Application of cyano-containing diphenylamine compound to preparation of antitumor drugs
A technology containing cyanodiphenylamine and anti-tumor drugs, which is applied in the field of anti-tumor drugs and medicine, and can solve the problems of no reports of anti-tumor drugs in compounds
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Embodiment 1
[0123] Embodiment 1: the preparation of table 6-1 compound
[0124]
[0125]Add 0.30 g (7.52 mmol) of sodium hydroxide to 0.35 g (3.76 mmol) of aniline in 40 ml of N,N-dimethylformamide, and slowly add 2,4,5,6-tetrachloro-1 , 3-phthalonitrile 1.00g (3.76mmol), after adding, continue to stir at room temperature for 5h, after TLC monitors the reaction, the reaction solution is poured into water, white solid is precipitated, suction filtration, and the filter cake is washed with 30ml water for two Once, washed twice with 20ml of petroleum ether, and dried to obtain 1.65g of the product, which is the compound in Table 6-1. Off-white solid, melting point 226-228°C.
[0126] 1 H-NMR (300MHz, internal standard TMS, solvent CDCl 3 ) δ (ppm): 7.22 (d, 2H, Ph-2, 6-2H, J = 7.5 Hz), 7.40-7.46 (m, 3H, Ph-3, 4, 5-3H).
Embodiment 2
[0127] Embodiment 2: the preparation of table 6-33 compound
[0128]
[0129] To a solution of 1.03g (8mmol) 2,6-difluoroaniline in 40ml N,N-dimethylformamide, add 0.64g (16mmol) of sodium hydroxide, and slowly add 2,4,5,6- Tetrachloro-1,3-benzenedicarbonitrile 2.13g (8mmol), after adding, continue stirring at room temperature for 5h, after TLC monitors the reaction, pour the reaction solution into water, extract with ethyl acetate, and wash the organic phase with water successively. Wash with saturated brine, dry, filter, precipitate, and purify the residue by column chromatography (eluent is ethyl acetate and petroleum ether (boiling range 60-90°C), volume ratio is 1:4) to obtain 1.65 g of the product, namely Table 6-33 Compounds. Pale yellow solid, melting point 264-266°C.
[0130] 1 H-NMR (300MHz, internal standard TMS, solvent CDCl 3 ) δ (ppm): 6.70 (s, 1H, NH), 7.07 (t, 2H, Ph-3, 5-2H, J = 8.1 Hz), 7.37 (m, 1H, Ph-4-1H).
Embodiment 3
[0131] Embodiment 3: the preparation of table 6-39 compound
[0132]
[0133] The synthesis method is the same as that of the compound in Table 6-1, a brownish black solid with a melting point of 209-212°C.
[0134] 1 H-NMR (300MHz, internal standard TMS, solvent CDCl 3 )δ (ppm): 6.95 (s, 1H, NH), 7.20 (d, 1H, Ph-6-H, J=8.1Hz), 7.36 (dd, 1H, Ph-5-H, 3 J=8.7Hz, 4 J = 2.7 Hz), 7.54 (d, 1H, Ph-3-H, J = 2.4 Hz).
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