Novel method for synthesizing N-substitute amide derivative
A technology of amide derivatives and a new method, which is applied in the preparation of organic compounds, the formation/introduction of amide groups, the preparation of carboxylic acid amides, etc., can solve the problems of high reaction temperature, limited substrate range, cumbersome operation process, etc. Simple operation, easy product separation and high reaction efficiency
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Embodiment 1
[0036]
[0037] At room temperature, add 0.2 mmol of the compound represented by formula (I-1) and 1 ml of formamide into a reaction tube equipped with a stirring magnet, stir and raise the temperature to 120° C., and react at this temperature for 15 h.
[0038] After the reaction, the reaction solution was cooled to room temperature, 15ml of ethyl acetate and 15ml of water were added, the organic layer was washed with 15ml of saturated ammonium chloride solution and 15ml of saturated sodium chloride solution, dried over anhydrous sodium sulfate for 1 hour, and covered with a layer of Silica gel funnel was used for filtration, and then the solvent was distilled off under reduced pressure, and the residue was purified by thin-layer chromatography silica gel plate (20cm×20cm) to obtain the target product represented by formula (III-1).
[0039] After calculation, the yield of the target product represented by formula (III-1) is 99%.
[0040] NMR data: 1 H NMR (500MHz, CDCl ...
Embodiment 2
[0043]
[0044] At room temperature, add 0.2 mmol of the compound represented by formula (I-2) and 1 ml of formamide into a reaction tube equipped with a stirring magnet, stir and raise the temperature to 120° C., and react at this temperature for 15 h.
[0045] After the reaction, the reaction solution was cooled to room temperature, 15ml of ethyl acetate and 15ml of water were added, the organic layer was washed with 15ml of saturated ammonium chloride solution and 15ml of saturated sodium chloride solution, dried over anhydrous sodium sulfate for 1 hour, and covered with a layer of Silica gel funnel was used for filtration, and then the solvent was distilled off under reduced pressure, and the residue was purified by thin-layer chromatography silica gel plate (20cm×20cm) to obtain the target product represented by formula (III-2).
[0046] After calculation, the yield of the target product represented by formula (III-2) is 74%.
[0047] NMR data: 1 H NMR (500MHz, CDCl 3 ...
Embodiment 3
[0050]
[0051] At room temperature, add 0.2 mmol of the compound represented by formula (I-3) and 1 ml of formamide into a reaction tube equipped with a stirring magnet, stir and raise the temperature to 120° C., and react at this temperature for 15 h.
[0052] After the reaction, the reaction solution was cooled to room temperature, 15ml of ethyl acetate and 15ml of water were added, the organic layer was washed with 15ml of saturated ammonium chloride solution and 15ml of saturated sodium chloride solution, dried over anhydrous sodium sulfate for 1 hour, and covered with a layer of Silica gel funnel was used for filtration, and then the solvent was distilled off under reduced pressure, and the residue was purified by thin-layer chromatography silica gel plate (20cm×20cm) to obtain the target product represented by formula (III-3).
[0053] After calculation, the yield of the target product represented by formula (III-3) is 55%.
[0054] NMR data: 1 H NMR (500MHz, CDCl ...
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