Process for synthesizing acylations enamine
A technology of acylating enamines and synthesis methods, applied in chemical instruments and methods, organic chemistry, chemical/physical processes, etc., can solve problems such as unfriendly environment, long reaction time, hidden safety hazards, etc., and achieve environmental friendliness and easy operation , the effect of mild conditions
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Embodiment 1
[0016]
[0017] Dicarbonyl compound 1a (5mmol, 500mg) and amine compound 2a (5.5mmol, 512mg) in pure water (6m1), add 0.005 equivalent of phosphotungstic acid (0.025mmol, 72mg) and stir at 25°C (ie, room temperature) for reaction 12 Hour. After the reaction was completed, the reaction solution was extracted with ethyl acetate, the organic layers were combined, the liquid was separated and the water layer was discarded; the organic layer was washed successively with saturated sodium carbonate solution and saturated sodium chloride solution, dried over anhydrous magnesium sulfate, filtered, and precipitated under reduced pressure. A crude product was obtained; the crude product was separated by column chromatography to obtain a white solid 3a (630 mg, 72%).
[0018] Attached: 3a: 1 H NMR (CDCl 3 ): d 2.289 (s, 3H, CH 3 ), 2.294 (s, 3H, CH 3 ), 6.00(s, 1H, CH), 7.37-7.42(m, 4H, Ph). 13 C NMR (CDCl 3 ): d 12.62, 13.70, 107.57, 125.99, 129.34, 133.04, 138.74, 139.60, 149.5...
Embodiment 2
[0020]
[0021] Dicarbonyl compound 1a (5mmol, 500mg) and amine compound 2a (5.5mmol, 512mg) in pure water (6ml), add 0.01 equivalent of phosphotungstic acid (0.05mmol, 114mg) and stir at 25°C (ie, room temperature) for 12 hours. . After the reaction was completed, the reaction solution was extracted with ethyl acetate, the organic layers were combined, the liquid was separated and the water layer was discarded; the organic layer was washed successively with saturated sodium carbonate solution and saturated sodium chloride solution, dried over anhydrous magnesium sulfate, filtered, and precipitated under reduced pressure. A crude product was obtained; the crude product was separated by column chromatography to obtain 3a (788 mg, 90%) as a white solid.
Embodiment 3
[0023]
[0024] Dicarbonyl compound 1a (5mmol, 500mg) and amine compound 2a (5.5mmol, 512mg) in pure water (6ml), add 0.015 equivalent of phosphotungstic acid (0.075mmol, 216mg) and stir at 25°C (ie, room temperature) for 12 hours. . After the reaction was completed, the reaction solution was extracted with ethyl acetate, the organic layers were combined, the liquid was separated and the water layer was discarded; the organic layer was washed successively with saturated sodium carbonate solution and saturated sodium chloride solution, dried over anhydrous magnesium sulfate, filtered, and precipitated under reduced pressure. A crude product was obtained; the crude product was separated by column chromatography to obtain 3a (788 mg, 90%) as a white solid.
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