4-methyl-1h-diaryl pyrromonazole derivative and medicament usage thereof
A technology of diarylpyrazoles and derivatives, which is applied in the directions of drug combinations, medical preparations containing active ingredients, pharmaceutical formulas, etc., can solve the problems of easy tolerance and addiction, restricted use and the like
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Embodiment 1
[0059] Example 1 1-(2,4-dichlorophenyl)-5-(4-chlorophenyl)-N-(2-9H-fluorenyl)-4-methyl-1H-pyrazole-3-methyl Preparation of amides.
[0060]
[0061] Step 1 Preparation of 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-methylpyrazole-3-carbonyl chloride.
[0062] Take 0.5g of 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-methylpyrazole-3-carboxylic acid, dissolve it in 10ml of toluene, add 0.29ml of thionyl chloride, Heat to reflux. After 4 hours, distill off the thionyl chloride and toluene, then add 10ml of toluene three times, and distill to obtain 0.4g of reddish-brown oil. Feed directly to the next step reaction.
[0063] Step 2 1-(2,4-dichlorophenyl)-5-(4-chlorophenyl)-N-(2-9H-fluorenyl)-4-methyl-1H-pyrazole-3-carboxamide preparation.
[0064] The formyl chloride obtained in the previous step was dissolved in 4 ml of dichloromethane, slowly added dropwise to a solution of 0.23 g of 2-aminofluorene and 0.234 ml of triethylamine in 5 ml of dichloromethane at 0°C, and reac...
Embodiment 2
[0066] Example 2 N-(4-bromophenyl)-1-(2,4-dichlorophenyl)-5-(4-chlorophenyl)-4-methyl-1H-pyrazole-3-carboxamide preparation.
[0067]
[0068] Refer to Example 1 for the preparation method of 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-methylpyrazole-3-carbonyl chloride.
[0069] The obtained formyl chloride was dissolved in 4ml of dichloromethane, slowly added dropwise to a solution of 0.215g of p-bromoaniline and 0.234ml of triethylamine in 5ml of dichloromethane at 0°C, and reacted at room temperature for 9 hours. Separation with petroleum ether: ethyl acetate = 2: 1 column chromatography to obtain 0.327 g of N-(4-bromophenyl)-1-(2,4-dichlorophenyl)-5-(4-chlorobenzene base)-4-methyl-1H-pyrazole-3-carboxamide, mp: 157.6-159.3°C, two-step total yield 46.58%,
[0070] 1 H-NMR (DMSO, δppm): 2.29 (s, 3H), 7.26 (dd, 2H), 7.47-7.51 (m, 5H), 7.79-7.83 (m, 4H), 10.35 (s, 1H). FAB-MS (m / e): 536.0 (M + ).
Embodiment 3
[0071] Example 3 1-(2,4-dichlorophenyl)-5-(4-chlorophenyl)-4-methyl-N-(3-pyridyl)-1H-pyrazole-3-carboxamide preparation.
[0072]
[0073] Refer to Example 1 for the preparation method of 5-(4-chlorophenyl)-1-(2,4-dichlorophenyl)-4-methylpyrazole-3-carbonyl chloride.
[0074] The obtained formyl chloride was dissolved in 4ml of dichloromethane, slowly added dropwise to a solution of 0.141g of p-bromoaniline and 0.234ml of triethylamine in 5ml of dichloromethane at 0°C, and reacted at room temperature for 6.5 hours. Using petroleum ether: ethyl acetate = 1:3 column chromatography to obtain 0.311g of 1-(2,4-dichlorophenyl)-5-(4-chlorophenyl)-4-methyl-N- (3-pyridyl)-1H-pyrazole-3-carboxamide mp: 162.8-164.1°C, two-step total yield 51.86%,
[0075] 1 H-NMR (DMSO, δppm): 2.31 (s, 3H), 7.27-7.38 (m, 3H), 7.47 (d, 2H), 7.60 (dd, 1H), 7.80-7.84 (m, 2H), 8.22- 8.30(m, 2H), 8.98(d, 1H), 10.47(s, 1H).FAB-MS(m / e): 457.0(M + ).
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