1-aryl-2-acetone compound preparation method
A compound, aryl acrylic acid technology, applied in the field of 1-aryl-2-acetone compound synthesis, can solve the problems of high explosiveness, complicated operation, long steps, etc., and achieves reduction of reaction steps, improved operation safety, operation The effect of process coherence
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Embodiment 1
[0038] 30.0g (184.97mmol) of (E)-2-methyl-3-phenylacrylic acid, 200mL of toluene, 51.9g (188.67mmol) of DPPA and 19.6g (194.22mmol) of triethylamine were successively added to a 500mL reaction flask, The reaction was stirred at 25 °C for 30 min; the temperature was raised to 110 °C for 1 h; 100 mL of concentrated hydrochloric acid was added to the reaction solution, and the reaction was continued for 1 h. The reaction solution was cooled to room temperature, the organic layer was separated, the organic layer was washed with saturated sodium carbonate solution, and the toluene was evaporated under reduced pressure to obtain a yellow oily liquid. . The product is analyzed by gas chromatography, and the purity is over 99.5%. 1H NMR (CDCl 3, 300MHz): δ (ppm) 7.22-7.39 (m, 5H), 3.71 (s, 2H), 2.17 (s, 3H); 13C NMR (CDCl 3 , 101MHz): δ (ppm) 206.3, 134.3, 129.4, 128.8, 127.1, 51.0, 29.3; GC-MS (EI) found 134.2 [M + ].
Embodiment 2
[0040] (E)-2-methyl-3-(4-methoxyphenyl)acrylic acid 30.0 g (156.08 mmol), toluene 200 mL, DPPA 43.8 g (159.20 mmol) and triethylamine 16.6 g (163.88 mmol) were sequentially It was added to a 500 mL reaction flask, and the reaction was stirred at 25 °C for 30 min; the temperature was raised to 110 °C for 1.5 h; 100 mL of concentrated hydrochloric acid was added to the reaction solution, and the reaction was continued for 1 h. The reaction solution was cooled to room temperature, the organic layer was separated, the organic layer was washed with saturated sodium carbonate solution, and the toluene was evaporated under reduced pressure to obtain a yellow oily liquid. The crude product was rectified to obtain 1-(4-methoxyphenyl)-2-propanone 21.8g, 85% yield. The product is analyzed by gas chromatography, and the purity is over 99.5%. GC-MS(EI) found 164.1[M + ].
Embodiment 3
[0042] (E)-2-methyl-3-(3,4-dimethoxyphenyl)acrylic acid 30.0 g (134.99 mmol), toluene 200 mL, DPPA 37.9 g (137.69 mmol) and triethylamine 14.3 g (141.74 mmol) mmol) were sequentially added to a 500 mL reaction flask, and the reaction was stirred at 25 °C for 1 h; the temperature was raised to 110 °C for 1.5 h; 100 mL of concentrated hydrochloric acid was added to the reaction solution, and the reaction was continued for 1.5 h. The reaction solution was cooled to room temperature, the organic layer was separated, the organic layer was washed with saturated sodium carbonate solution, and the toluene was evaporated under reduced pressure to obtain a yellow oily liquid. The crude product was rectified to obtain 1-(4-methoxyphenyl)-2-propanone 21.5g, yield 82%. The product is analyzed by gas chromatography, and the purity is over 99.5%. GC-MS(EI)found 194.1[M + ].
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