Sulfonamide compound, preparation method, and applications thereof
A technology of compounds and oxides, applied in the field of medicine
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preparation example 1
[0211] Intermediate Preparation Example 1: Preparation of N-ethyl-N-(3-hydroxy-2,3-dihydro-1H-inden-5-yl)-3-(trifluoromethyl)benzenesulfonamide
[0212]
[0213] Step 1: Preparation of N-(3-oxo-2,3-dihydro-1H-inden-5-yl)-3-(trifluoromethyl)benzenesulfonamide
[0214] Add 6-amino-1-indanone (8.5g, 57.8mmol) and 3-trifluoromethylbenzenesulfonyl chloride (15.5g, 63.6mmol) into pyridine (100mL) and heat to 55°C for 12 hours. The reaction solution was concentrated under reduced pressure, poured into water (500mL), extracted three times with ethyl acetate, combined the organic phases, dried over anhydrous sodium sulfate, filtered and concentrated the filtrate under reduced pressure to obtain the title compound of this step (19.4g, yield : 94.5%).
[0215] MS m / z(ESI):373.1[M+NH 4 ] + .
[0216] The second step: the preparation of N-ethyl-N-(3-oxo-2,3-dihydro-1H-inden-5-yl)-3-(trifluoromethyl)benzenesulfonamide
[0217] N-(3-oxo-2,3-dihydro-1H-inden-5-yl)-3-(trifluoromethyl)ben...
Embodiment 1
[0223] Example 1: N-(3-(2-chloro-6-(trifluoromethyl)phenoxy)-2,3-dihydro-1H-inden-5-yl)-N-ethyl-3- (Trifluoromethyl)benzenesulfonamide (Compound 1)
[0224]
[0225] Triphenylphosphine (204.2 mg, 778.4 μmol), N-ethyl-N-(3-hydroxy-2,3-dihydro-1H-inden-5-yl)-3-(trifluoromethyl)benzene Sulfonamide (100mg, 259.5μmol) and 2-chloro-6-trifluoromethylphenol (76.5mg, 389.2μmol) were mixed in a 100mL reaction flask, under nitrogen protection, anhydrous tetrahydrofuran (5mL) was added, and stirred in an ice bath for 0.5 hours Finally, a solution of diisopropyl azodicarboxylate (157.4 mg, 778.4 μmol) in anhydrous tetrahydrofuran (1 mL) was added, stirring was continued for 0.5 hours in an ice bath, and the reaction was continued at room temperature for about 2 hours. The reaction solution was concentrated and poured into water (100 mL), extracted three times with ethyl acetate, the organic phases were combined, dried over anhydrous sodium sulfate, filtered and the filtrate was concent...
Embodiment 2
[0228] Example 2: N-(3-(2-cyanophenoxy)-2,3-dihydro-1H-inden-5-yl)-N-ethyl-3-(trifluoromethyl)benzenesulfonate Amide (compound 2)
[0229]
[0230] Using the synthetic route of Example 1, replacing the raw material 2-chloro-6-trifluoromethylphenol with 2-cyanophenol, the title compound (52.0 mg, yield: 33.4%) was obtained.
[0231] MS m / z(ESI):504.1[M+NH 4 ] + .
[0232] 1 H-NMR (400MHz, CDCl 3 )δ:8.08-8.06(m,1H),7.87-7.79(m,3H),7.74-7.66(m,2H),7.45-7.43(m,1H),7.38-7.36(m,1H),7.15- 7.11(m,1H),7.04-7.02(m,2H),5.97-5.94(m,1H),3.65-3.52(m,2H),3.11-3.06(m,1H),2.96-2.92(m,1H ), 2.69-2.61 (m, 1H), 2.15-2.07 (m, 1H), 0.96 (t, J=8.0Hz, 3H).
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