Acyl chloride and sulfonyl chloride derivant, and uses thereof
A compound and acetamide technology, applied in the field of acyl chloride and sulfonyl chloride isoxazoline derivatives and their preparation, can solve the problems of difficult clinical treatment, bacterial resistance and the like
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[0071] Reference example 1 (preparation of compound 6)
[0072]
[0073] Using 3,4-difluorobenzaldehyde as the starting material, react with hydroxylamine hydrochloride under strong alkaline conditions to generate 3,4-difluorobenzoxime, and then react with N-chlorosuccinimide to generate 3,4 - Chloride of difluorobenzoxime, followed by cyclization with allyl acetamide to generate (±)-N-5-(acetamidomethyl)-3-(3,4-difluorophenyl)isoxazoline , after reacting with anhydrous piperazine to generate (±)-N-[[3-[3-fluoro-4-(1-piperazinyl)phenyl]-4,5-dihydro-5-isoxazolyl ]methyl]acetamide (compound 6). m.p.160.2-161.3℃, HPLC99.7%, 1 H-NMR (DMSO-d 6 , 400MHz) δ: 8.11-8.08 (1H, t, NH), 7.377-7.337 (2H, m, ArH), 7.057-7.013 (1H, t, ArH), 4.722-4.650 (1H, m, CH), 3.458 -3.349(1H, m), 3.239-3.210(2H, t), 3.089-3.029(1H, m), 2.982-2.959(4H, t), 2.833-2.822(4H, d), 2.494-2.458(1H, t), 1.085 (3H, s).
Embodiment 1
[0075] (±)-N-[[3-[3-fluoro-4-[4-(p-fluorophenylacetyl)-1-piperazinyl]phenyl]-4,5-dihydro-5-isoxazole Base] methyl] acetamide (compound I-1)
[0076]
[0077] In a 100ml three-necked round-bottomed flask, add 3.7g of compound 6, 40ml of chloroform, and 5g of anhydrous potassium carbonate, cool in an ice bath to -5°C, and add 2.1g of p-fluorophenylacetyl chloride in portions under stirring, keeping The temperature is below 15°C. After the addition, it was raised to room temperature, reacted for about 30 minutes, and then slowly raised to reflux, reacted for about 2.5 hours, and was monitored by TLC to complete the reaction. Add 50ml of water to wash, separate the organic layer, dry over anhydrous sodium sulfate, and distill under reduced pressure to obtain 3.97g of white solid (I-1), Rf=0.48 (developing solvent: dichloromethane / anhydrous methanol (v:v)= 19:1), m.p.196.6-197.8°C, HPLC 98.4%.
Embodiment 2-8
[0079] Referring to the operation of Example 1, the difference is that an acid chloride compound with a different structure is used instead of p-fluorophenylacetyl chloride in Example 1, and reacted with compound 6 to obtain the following compound of formula I.
[0080]
[0081]
[0082] The physical and chemical constants of the obtained general formula I compound are as follows:
[0083] I-2: white solid, yield 52.8%. m.p.197.8-198.6°C, Rf=0.74 (developing solvent: dichloromethane / anhydrous methanol (v:v)=19:1), HPLC 98.8%.
[0084] I-3: white solid, yield 57.2%. m.p.199.81-200.9°C, Rf=0.52 (developing solvent: dichloromethane / anhydrous methanol (v:v)=19:1), HPLC 98.3%.
[0085] I-4: Pale yellow solid, yield 72.6%. m.p.143.2-144.9°C, Rf=0.55 (developing solvent: dichloromethane / anhydrous methanol (v:v)=19:1), HPLC 99.1%.
[0086] I-5: white solid, yield 74.1%. m.p.185.9-186.9°C, Rf=0.65 (developing solvent: dichloromethane / anhydrous methanol (v:v)=19:1), HPLC 98.6%....
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