El-Salam Osama I Abd, Alsayed Ali S, Ali Korany A, Elwahab Ahmed A Abd, El-Galil E Amr Abd, Awad Hassan M
Applied Organic Chemistry Department, National Research Centre, Dokki, Giza 12622, Egypt.
Chemistry Department, Al-Azhar University, Nasr City, Cairo 1435, Egypt.
Molecules. 2015 Nov 16;20(11):20434-47. doi: 10.3390/molecules201119701.
A series of novel benzosuberone derivatives were synthesized and evaluated as antimicrobial agents by using substituted benzosuberone derivatives 1a,b as starting materials. Treatment of 1a,b with phenyl isothiocyanate in dimethylformamide was followed by treatment with cold HCl solution to afford the thioamides 4a,b, which was reacted with methyl iodide to obtain methylated products 5a,b. Cyclocondensation of 4a,b with chloroacetone 6 and phenacyl chloride 7 gave the corresponding thiophene derivatives 9a-c. Reaction of 4a,b with C-acetyl-N- arylhydrazonoyl chlorides 14a and 14b in boiling EtOH in the presence of triethylamine, afforded the corresponding 1,3,4-thiadiazoline derivatives 16a-d. The thioamides 4a,b were reacted with C-ethoxycarbonyl-N-arylhydrazonoyl chlorides 18a,b which afforded 1,3,4-thiadiazoline derivatives 19a-d. The benzosuberones 1a,b were treated with 3-mercaptopropanoic acid to give compounds 21a,b, which were cyclized to tricyclic thiopyran-4(5H)-one derivatives 22a,b. The latter compounds 22a,b were reacted with 3-mercaptopropanoic acid to give compounds 23a,b, which were cyclized tetracyclic ring systems 24a,b. Finally, compounds 24a,b were oxidized using hydrogen peroxide under reflux conditions to afford the oxidized form of the novel tetracyclic heterogeneous ring systems 25a,b. The newly synthesized compounds were screened for antimicrobial activities. The structures of new compounds were characterized by ¹H-NMR, 13C-NMR, IR, and EI-MS.
以取代苯并环庚酮衍生物1a、b为起始原料,合成了一系列新型苯并环庚酮衍生物,并对其作为抗菌剂进行了评估。1a、b与异硫氰酸苯酯在二甲基甲酰胺中反应,然后用冷盐酸溶液处理,得到硫代酰胺4a、b,其与碘甲烷反应得到甲基化产物5a、b。4a、b与氯丙酮6和苯甲酰氯7进行环缩合反应,得到相应的噻吩衍生物9a - c。4a、b与C - 乙酰基 - N - 芳基肼基酰氯14a和14b在沸腾的乙醇中,在三乙胺存在下反应,得到相应的1,3,4 - 噻二唑啉衍生物16a - d。硫代酰胺4a、b与C - 乙氧基羰基 - N - 芳基肼基酰氯18a、b反应,得到1,3,4 - 噻二唑啉衍生物19a - d。苯并环庚酮1a、b用3 - 巯基丙酸处理得到化合物21a、b,其环化得到三环噻喃 - 4(5H) - 酮衍生物22a、b。后一种化合物22a、b与3 - 巯基丙酸反应得到化合物23a、b,其环化得到四环体系24a、b。最后,化合物24a、b在回流条件下用过氧化氢氧化,得到新型四环杂环体系的氧化形式25a、b。对新合成的化合物进行了抗菌活性筛选。通过¹H - NMR、13C - NMR、IR和EI - MS对新化合物的结构进行了表征。