Chemical Data Collections Pub Date : 2021-02-21 , DOI: 10.1016/j.cdc.2021.100664 Pravinkumar Patil , Amjad Khan Pathan , Sainath Zangade
Present work deals with the synthesis of the 1-(4-bromo-1-hydroxynaphthalen-2-yl)ethan-1-one 3 from 2-acetyl-1-naphthol 2 using Br2/AcOH (20%) as brominating agent. The structure compound 3 was confirmed on the basis of spectral study such as FTIR, 1H NMR, 13C NMR and GCMS. The crystal structure of 4-bromo-2-acetyl-1-naphthol was also confirmed by the X-ray single-crystal diffractometry analysis and revealed the unit cell parameters, packing style. The single crystal has been grown by slow evaporation method at ambient temperature. The crystal size for compound 3 was found to be 0.150 × 0.120 × 0.100 mm3. The crystal has grown with monoclinic crystal system with Z value of four and space group symmetry was P21/c. The unit cell parameters and angles were a; 7.3584 Å, b; 17.772 Å, c; 8.357 Å, α; 90°, β; 108.711°, √; 90°. The crystal structure of 3 is stabilized via one strong classical hydrogen bond interaction and two weak intermolecular hydrogen bonding. The observed average bond lengths of CC, CH, CO, CBr and OH bonds were 1.410, 0.941, 1.289, 1.899 and 0.80 Å respectively.
中文翻译:
2-乙酰基-1-萘酚溴代衍生物的制备,光谱表征和单晶分析
目前的工作涉及使用Br 2 / AcOH(20%)作为溴化剂由2-乙酰基-1-萘酚2合成1-(4-溴-1-羟基萘-2-基)乙烷-1-酮3。根据诸如FTIR,1 H NMR,13 C NMR和GCMS的光谱研究确认了结构化合物3。X射线单晶衍射分析也证实了4-溴-2-乙酰基-1-萘酚的晶体结构,并揭示了晶胞参数,堆积方式。单晶已经通过在环境温度下的缓慢蒸发法生长。发现化合物3的晶体尺寸为0.150×0.120×0.100mm 3 。晶体以单斜晶体系统生长,Z值为4,空间群对称性为P21 / c。晶胞参数和角度为a; 7.3584Å,b; 17,772Å,c; 8.357Å,α; 90°,β;108,711°,√; 90°。的晶体结构3被稳定经由一个强经典的氢键相互作用和两个弱的分子间氢键键合。观察到的C C,C H,C O,C Br和O H键的平均键长分别为1.410、0.941、1.289、1.899和0.80Å。