N-benzyl quinoline carboxylic acid compound, combination and preparation method thereof
A compound, benzyl technology, applied in the field of N-benzyl quinoline carboxylic acid compounds
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Embodiment 1
[0101] Preparation of 2-(6-methyl-1-benzyl-4-oxo-1,4-dihydroquinolin-3-yl)acetic acid
[0102] The title compound was prepared according to the method of the following Scheme 1
[0103] Process 1
[0104]
[0105] (i) Preparation of 3-(4-methylanilino) propionic acid
[0106] Add 21.4g (0.2mol) of p-methylaniline, 22.0g (0.22mol) of ethyl acrylate and 1.0mL of glacial acetic acid into a 250mL round bottom bottle, heat up to reflux, and stir for 15 hours. After the reaction was completed, the remaining ethyl acrylate was distilled off under reduced pressure, 100 mL of 20% aqueous sodium hydroxide solution was added to the reaction solution, and the temperature was raised to reflux and the reaction was stirred for 30 minutes. After the reaction, the reaction solution was cooled to room temperature, and an equal volume of water was added. Extract with 180ml of ethyl acetate (60mL×3), adjust the water phase to pH 6-7 with concentrated hydrochloric acid, then adjust the pH to...
Embodiment 12
[0120] Preparation of 2-(6-fluoro-1-benzyl-4-oxo-1,4-dihydroquinolin-3-yl)acetic acid (compound 12)
[0121] The title compound was prepared according to the method of the following Scheme 2
[0122] Process 2
[0123]
[0124] (i) Preparation of 3-(4-fluoroanilino) propionic acid
[0125] Add 16.65 g (0.15 mol) of fluoroaniline, 16.5 g (0.165 mol) of ethyl acrylate and 1.0 mL of glacial acetic acid into a 250 mL round bottom bottle, raise the temperature to reflux, and stir for 15 hours. After the reaction was completed, the remaining ethyl acrylate was distilled off under reduced pressure, 100 mL of 20% aqueous sodium hydroxide solution was added to the reaction solution, and the temperature was raised to reflux and the reaction was stirred for 30 minutes. After the reaction, cool the reaction solution to room temperature, add an equal volume of water; extract with 150ml ethyl acetate (50mL×3), adjust the water phase to pH 6-7 with concentrated hydrochloric acid, and th...
Embodiment 23
[0139]Preparation of 2-(6-methoxy-1-benzyl-4-oxo-1,4-dihydroquinolin-3-yl)acetic acid (compound 27)
[0140] The title compound was prepared according to the method of the following Scheme 3
[0141] Process 3
[0142]
[0143] (i) Preparation of 3-(4-methoxyanilino) propionic acid
[0144] Add 18.45 g (0.15 mol) of p-methoxyaniline, 16.5 g (0.165 mol) of ethyl acrylate and 1.0 mL of glacial acetic acid into a 250 mL round-bottomed bottle, stir and react at 50°C for 15 hours. After the reaction was completed, the remaining ethyl acrylate was distilled off under reduced pressure, 100 mL of 20% aqueous sodium hydroxide solution was added to the reaction solution, and the temperature was raised to reflux and the reaction was stirred for 30 minutes. After the reaction, the reaction solution was cooled to room temperature, and an equal volume of water was added. Extract with 150ml of ethyl acetate (50mL×3), adjust the water phase to pH 6-7 with concentrated hydrochloric acid,...
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