Amide derivatives, their preparation method and their use in medicine
A technology of use and medicine, applied in the field of amide derivatives, their preparation and their use in medicine
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Embodiment 1
[0138] (R)-1-(4-((S)-1-(3,5-Dimethyl-4-(4-(trifluoromethyl)-1H-pyrazol-1-yl)phenoxy) Butyl)benzoyl)piperidine-3-carboxylic acid
[0139]
[0140] first step
[0141] Methyl 4-(1-hydroxybutyl)benzoate
[0142] Methyl p-formylbenzoate 1a (10.0 g, 60.92 mmol) was dissolved in 100 mL of tetrahydrofuran, and propylmagnesium bromide (33.5 mL, 67.0 mmol) was added at -78°C, and reacted at room temperature for 3 hours. Add 300mL of ethyl acetate, wash with saturated ammonium chloride solution (200mL) and saturated sodium chloride solution (200mL), the organic phase is dried over anhydrous sodium sulfate, concentrated under reduced pressure, and the obtained residue is subjected to silica gel column chromatography ( Eluent: petroleum ether: ethyl acetate system) purification to obtain 4-(1-hydroxybutyl)methyl benzoate 1b (8.66g, colorless liquid), yield: 68.0%
[0143] MS m / z(ESI): 209.0[M+1]
[0144] second step
[0145] Methyl 4-butyrylbenzoate
[0146] Dissolve methyl 4-(1-...
Embodiment 2
[0170] (R)-1-(4-((S)-1-(3,5-Dimethyl-4-(4-(trifluoromethyl)-1H-pyrazol-1-yl)phenoxy) Butyl)-2-fluorobenzoyl)piperidine-3-carboxylic acid
[0171]
[0172] first step
[0173] Methyl 2-fluoro-4-(1-hydroxybutyl)benzoate
[0174] Methyl 2-fluoro-4-formylbenzoate 2a (3.0g, 16.5mmol) was dissolved in 60mL of tetrahydrofuran, under nitrogen protection, under stirring at -78°C, slowly added propylmagnesium bromide (8.6mL, 17.3mmol) , react at room temperature for 2 hours. The reaction solution was cooled to 0°C, and saturated ammonium chloride solution (30 mL) was slowly added, extracted with ethyl acetate (20 mL x3), the organic phase was dried over anhydrous sodium sulfate, concentrated under reduced pressure, and the obtained residue was subjected to silica gel column chromatography method (eluent: petroleum ether: ethyl acetate system) to obtain 2-fluoro-4-(1-hydroxybutyl)methyl benzoate 2b (850mg, colorless liquid), yield: 23.0%
[0175] 1 H NMR (400MHz, CDCl 3):δ7.86(d...
Embodiment 3
[0202] (S)-1-(4-((S)-1-(3,5-Dimethyl-4-(4-(trifluoromethyl)-1H-pyrazol-1-yl)phenoxy) Butyl)-2-fluorobenzoyl)piperidine-3-carboxylic acid
[0203]
[0204] first step
[0205] (S)-1-(2-fluoro-4-(R)-1-hydroxybutyl)benzoylpiperidinyl)-3-carboxylic acid ethyl ester
[0206] (R)-2-fluoro-4-(1-hydroxybutyl)benzoic acid 2e (150mg, 0.71mmol), (S)-piperidine-3-carboxylic acid ethyl ester 3a (142uL, 0.92mmol), bis( 2-oxo-3-oxazolidinyl)phosphoryl chloride (270mg, 1.06mmol) and N,N-diisopropylethylamine (0.50mL, 2.82mmol) were dissolved in 5mL tetrahydrofuran, and the reaction solution was heated at room temperature React for 2 hours. The reaction solution was concentrated under reduced pressure, and the obtained residue was purified by silica gel column chromatography (developing solvent: petroleum ether: ethyl acetate system) to obtain (S)-1-(2-fluoro-4-(R)-1 -Hydroxybutyl)benzoylpiperidinyl)-3-carboxylic acid ethyl ester 3b (250 mg, colorless liquid), yield: 99.0%.
[0207] MS...
PUM
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