Medicine for treating depression
A technology of pharmacy and compound, applied in the field of chemical medicine, can solve the problems of sexual dysfunction, low efficacy, suicidal tendency and so on
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Embodiment 1
[0027] Example 1: Synthesis of (E)-2-((3-(4-(trifluoromethyl)styryl)phenyl)thio)pyridine
[0028] 1-1. Synthesis of 1-iodo-3-nitrobenzene:
[0029]
[0030] Add 70mL of DMF to a 500mL reaction flask, then add nitrobenzene (30.12g, 0.245mol) and potassium carbonate (25.2g, 0.182mol), cool in an ice bath below 10°C, and after stirring, add iodine (0.250mol) Dissolve in 30mL DMF and add dropwise to the reaction system. The dropping time is 1 hour. The reaction mixture is stirred at 25°C for 16 hours until the reaction is complete. Sodium thiosulfate (22.3g, 0.141mol) and potassium carbonate (0.150g) are added. ) Aqueous solution (150mL), while maintaining the internal temperature below 30℃, stirring for 30 minutes, adding 200mL of water while stirring, the solid precipitated, suction filtration, the filter cake was washed with water, and vacuum dried at 60℃ for 12 hours to obtain a pale yellow solid 1-iodine -3-nitrobenzene, 43.84g, yield 72%. 1 H-NMR (400MHz, CDCl3) δ: 7.35 (t, 1H),...
Embodiment 2
[0043] Example 2: Synthesis of (E)-2-((3-(4-(trifluoromethyl)styryl)phenyl)thio)-6-fluoropyridine:
[0044]
[0045] Add 175mL DMF and (E)-1-iodo-3-(4-(trifluoromethyl)styryl)benzene (35.77g, 0.096mol) into a 500mL reaction flask, and add [1,1'- Bis(diphenylphosphine)ferrocene]dichloropalladium dichloromethane complex (1.49g, 0.0018mol), cesium carbonate (19.8g, 0.061mol) and dichloromethane 2mL, add 6-fluoro-pyridine -2-mercaptan (0.102mol), heated to 80℃, reacted for 16 hours until the reaction is complete, rotary evaporation to remove DMF, cooled to room temperature, add ethyl acetate 100mL, water 150mL, stir for 40 minutes, separate the organic phase, brine Wash, separate into layers, dry the organic phase with sodium sulfate, filter, evaporate to dryness, flash column chromatography to obtain pale yellow (E)-2-((3-(4-(trifluoromethyl)styryl)benzene (Yl)thio)-6-fluoropyridine, 29.16g, yield 81%. LC-MS (ESI, pos, ion) m / z: 376 [M+H].
Embodiment 3
[0046] Example 3: Synthesis of (E)-2-((3-(4-(trifluoromethyl)styryl)phenyl)sulfanyl)-6-methyl-pyridine:
[0047]
[0048] Add 175mL DMF and (E)-1-iodo-3-(4-(trifluoromethyl)styryl)benzene (35.77g, 0.096mol) into a 500mL reaction flask, and add [1,1'- Bis(diphenylphosphine)ferrocene]dichloropalladium dichloromethane complex (1.49g, 0.0018mol), cesium carbonate (19.8g, 0.061mol) and dichloromethane 2mL, add 6-methyl- Pyridine-2-thiol (0.102mol), heated to 80°C, reacted for 16 hours until the reaction was complete, rotary evaporated to remove DMF, cooled to room temperature, added ethyl acetate 100mL, water 150mL, stirred for 40 minutes, separated the organic phase, Wash with brine, separate the layers, dry the organic phase with sodium sulfate, filter, evaporate to dryness, flash column chromatography to obtain pale yellow (E)-2-((3-(4-(trifluoromethyl)styryl) Phenyl)sulfanyl)-6-methyl-pyridine, 31.70 g, yield 89%. LC-MS (ESI, pos, ion) m / z: 372 [M+H].
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