Signal channel inhibiting agent as well as preparation method and application thereof
A signal pathway and inhibitor technology, applied in the field of chemical medicine
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Embodiment 1
[0271] Example 1 2-chloro-N-(4-chloro-3-(pyridin-2-ylcarbamoyl)phenyl)-4-(methylsulfonyl)benzamide (compound 1)
[0272]
[0273] Step 1: Take 2.34g 2-chloro-4-methanesulfonylbenzoic acid, add 40mL SOCl 2 , reflux reaction for 1h, after the reaction, spin dry. Add 30 mL of DMAC and stir to dissolve. 1.716 g of 2-chloro-5-aminobenzoic acid was dissolved in 10 mL of DMAC and added dropwise to the previous solution, followed by the addition of 1 mL of triethylamine. React at 80°C for 5h, and monitor the reaction by TLC. After the reaction was over, 250 mL of distilled water was added to the reaction system, and a white solid was precipitated, which was filtered by suction and dried in vacuo to obtain 3.1 g of 2-chloro-5-(2-chloro-4-(methylsulfonyl)benzamido)benzoic acid. The rate is 79.8%. 1 H-NMR (DMSO-d 6 )δ:13.51(s,1H),10.97(s,1H),7.54-8.21(m,6H),3.31(s,3H);ESI-MS:387.99(M+H) + .
[0274] Step 2: Take 77.6mg of 2-chloro-5-(2-chloro-4-(methylsulfonyl)benzamido)benzoic...
Embodiment 2
[0275] Example 2 2-chloro-N-(4-chloro-3-(3-hydroxyphenyl-2-ylcarbamoyl)phenyl)-4-(methylsulfonyl)benzamide (compound 2)
[0276]
[0277] Take 77.7mg of 2-chloro-5-(2-chloro-4-(methylsulfonyl)benzamido)benzoic acid, 61.9mg of DCC, 27.1mg of HOBT, add 4mL of DMF to dissolve, stir at 0℃ for 1h, add 35 mg of 3-aminophenol was stirred at 0°C for 1 hour, and the temperature was raised to 80°C for 5 hours. Cool and filter with suction, add 10ml of 1M hydrochloric acid to the filtrate, then extract with ethyl acetate, dry over sodium sulfate, filter with suction, concentrate to dryness, and purify with silica gel column chromatography (EA:PE=1:2) to obtain 75.8mg of 2-chloro -N-(4-chloro-3-(3-hydroxyphenyl-2-ylcarbamoyl)phenyl)-4-(methylsulfonyl)benzamide (2), yield 79.1%. 1 H-NMR (DMSO-d 6 ,400MHz)δ:11.04(s,1H),10.47(s,1H),9.56(s,1H),8.16(s,1H),7.34-8.04(m,6H),7.11(s,2H),6.56 (s,1H),3.63(s,3H); 13 C-NMR (DMSO-d 6 ,100MHz)δ:165.0,164.5,162.9,158.1,143.6,141.2,140.2,137.9,131....
Embodiment 3
[0278] Example 3 2-chloro-N-(4-chloro-3-(2,3-dimethylphenyl-2-ylcarbamoyl)phenyl)-4-(methylsulfonyl)benzamide (compound 3)
[0279]
[0280] Take 77.4mg of 2-chloro-5-(2-chloro-4-(methylsulfonyl)benzamido)benzoic acid, 61.8mg of DCC, 27.2mg of HOBT, add 4mL of DMF to dissolve, stir at 0°C for 1h, add 38 mg of 2-aminopyridine was stirred at 0°C for 1 hour, then heated to 80°C for 5 hours. Cool and filter with suction, add 10ml of 1M hydrochloric acid to the filtrate, extract with ethyl acetate, dry over sodium sulfate, filter with suction, concentrate to dryness, and purify with silica gel column chromatography (EA:PE=1:2) to obtain 82.1mg of 2-chloro -N-(4-chloro-3-(2,3-dimethylphenyl-2-ylcarbamoyl)phenyl)-4-(methylsulfonyl)benzamide (3), yield 83.8% . 1 H-NMR (DMSO-d 6 ,600MHz)δ:11.02(s,1H),10.09(s,1H),8.17(s,1H),7.83-8.05(m,4H),7.58(d,1H,J=8.4Hz),7.21(d ,1H,J=7.2Hz),7.09-7.14(m,2H),3.41(s,3H); 13 C-NMR (DMSO-d 6 ,150MHz)δ:165.4,164.5,143.7,141.3,138.0,137.7,135.9,1...
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