5-amino-3,4-dihydro-2(1H)-quinolinone compounds as well as synthetic method and application thereof
A technology of quinolinones and dihydroquinolines, applied in organic chemistry, antibacterial drugs, antifungal agents, etc., can solve serious problems such as drug resistance, and achieve good antibacterial effects
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Embodiment 1
[0033] Embodiment 1: the preparation of compound 2
[0034]
[0035] Add 4.6 g (4.32 mmol, content 10%) of palladium carbon into 100 ml of isopropanol, and stir for 5 min. Weigh 13.6g (215.81mmol) of ammonium formate and add it into 20ml of water until it is completely dissolved, then add it into the above reaction solution. 7.0 g (43.16 mmol) of 5-amino-3,4-dihydroquinolin-2(1H)-one was added, 5.71 g (51.79 mmol) of 40% acetaldehyde aqueous solution was added dropwise, and the reaction was carried out at room temperature for 4 h. Suction filtration, the filtrate was spin-dried, 50ml of dichloromethane was added to dissolve the product, washed with saturated sodium chloride solution and water successively, and dried over anhydrous sodium sulfate. Spin-dry and dry to obtain 6.6 g of light yellow powdery solid, Mp=168-170° C., yield 80%.
Embodiment 2
[0036] Embodiment 2: the preparation of compound 3
[0037]
[0038] Weigh 26.5g (34.17mmol) of the compound and dissolve it in 100ml of methanol, then add 4.34g (34.17mmol) of zinc chloride, cool down to 0°C in an ice-salt bath, and add 4.1g of ethylene oxide dissolved in methanol cooled to 0°C (102.51mmol), react at room temperature for 10h. Rotary steaming, the obtained oily substance was successively added with 70ml of ethyl acetate, 30ml of water, and 15ml of ammonia water. After standing still, the layers were separated, and the aqueous layer was extracted twice with 50 ml and 25 ml of ethyl acetate in sequence, and the organic layers were combined and dried over anhydrous sodium sulfate. After spin-drying, 7.1 g of light yellow oil was obtained, with a yield of 89%.
Embodiment 3
[0039] Embodiment 3: the preparation of compound 4
[0040]
[0041]Weigh 3.5g (18.5mmol) of Boc-alanine and add it into 30ml of dichloromethane, then add 2.5g (18.5mmol) of 1-hydroxybenzotriazole and 0.21g (1.85mmol) of dimethylaminopyridine in sequence, N,N-dicyclohexylcarbodiimide 4.2g (20.35mmol), stirred for 0.5h. A solution of compound 34.33g (18.5mmol) in dichloromethane was added dropwise, and reacted at room temperature for 6h. Rotate to dryness, add 30ml of ethyl acetate, filter with suction, wash the filtrate with saturated sodium bicarbonate solution and water successively, and dry over anhydrous sodium sulfate. After spin-drying, 6.8 g of compound 4 was obtained as a yellow oil, with a yield of 90%.
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