Synthesis and characterization of novel 2-fluoro/chloro-3-pyridyl selenides: X-ray crystal structure of bis(2-fluoro-3-pyridyl) diselenide and bis(2-fluoro-3-pyridylseleno) methane
作者:Shivani Gulati (nee Doomra)、Kuldip K. Bhasin
DOI:10.1016/j.jfluchem.2013.07.007
日期:2013.12
An efficient one-pot synthesis of bis(2-fluoro/chloro-3-pyridyl) diselenide has been successfully achieved under dry-ice/acetone bath temperature that involves deprotonation of corresponding 2-fluoro/chloropyridine at C-3 with lithium di-isopropylamide, insertion of elemental selenium followed by the subsequent aerial oxidation. A series of novel and synthetically important unsymmetrical 2-fluoro/2-chloro
在干冰/丙酮浴温度下成功地完成了一锅法合成的双(2-氟/氯-3-吡啶基)二硒化物的有效反应,该过程涉及在相应的温度下在C-3下用二锂锂对相应的2-氟/氯吡啶进行去质子处理。异丙酰胺,插入元素硒,然后进行随后的空中氧化。通过标题化合物“ bis”的还原裂解,制备了一系列新颖且在合成上很重要的不对称的2-氟/ 2-氯取代的烷基/烯丙基/苄基吡啶基硒化合物和二硒缩醛双(2-氟-3-吡啶基硒代)甲烷。(2-氟/氯-3-吡啶基)二硒化物与硼氢化钠,然后用适当的烷基化剂淬灭。通过将2-卤代吡啶去质子化并插入元素硒,然后加入适当的烷基化剂,可以实现相同的目的。迄今未知的化合物已通过元素分析和各种光谱技术,即FT-IR,多核(1 H,13 C,19 F和77 Se)NMR和质谱法进行了全面表征。双(2-氟-3-吡啶基)二硒化物和双(2-氟-3-吡啶基硒代)甲烷的晶体结构已经通过单晶X射线衍射(XRD)确定。