点击关注,化学科讯!Raney Ni加氢,但是当分子内存在对加氢敏感的官能团,如:卤素(Cl, Br and I; F 对加氢不敏感),双键,三键时,我们不得不采用其他方法, 最为经典的要数在酸性条件下的铁粉的还原。含硫的还原剂如硫化钠、硫化胺、亚硫酸氢钠、连二亚硫酸钠等是在碱性或中性条件下选用的还原剂. 此类还原剂的特点是能使多硝基化合物中部分硝基还原为氨基。
General procedure and reaction conditions optimization:In a round bottomed flask the nitro-compound (0.7 mmol) and the tertiary amine (3.5 mmol) were dissolved into the dry solvent (5 mL) under magnetic stirring and nitrogen atmosphere. A solution of freshly distilled HSiCl3 (2.5 mmol) in 2 mL of dry solvent was prepared apart, and it was added drop-wise to the first solution over 10 minutes at 0 °C. After stirring the reaction mixture for 18 h, 5 mL of a saturated solution of NaHCO3 was added drop-wise and the biphasic mixture was allowed to stir for 30 min. The crude mixture was extracted with ethyl acetate, dried over Na2SO4, filtered and then dried under reduced pressure to afford the crude product.参考资料:Metal-Free Reduction of Aromatic and Aliphatic Nitro Compounds to Amines: A HSiCl3‑Mediated Reaction of Wide General Applicability, Org. Lett. 2015, 17, 3941−3943. END资料领取回复你需要资料的关键词,查看领取例:后台回复“ChemDraw ”领取破解版安装包回复“MestReNova”领取破解版安装包回复“EndNote X9.1 ”领取破解版安装包回复“有机化学”领取经典化学书籍回复“科研礼包”领取更多丰富所需资料回复“资料全集”领取5款破解版资料有偿征稿 本平台长期征稿,投稿请发至邮箱:tg@bcpmdata.com,目前仅接受原创首发类相关稿件或顶级化学外刊文献的前沿解读。来稿邮件标题:【微信投稿】+文章标题+作者、稿件请以附件方式发送,我们将从中挑选并发表在“化学科讯”微信公号。一经发表,稿酬丰厚,欢迎赐稿,期待佳作。 NO.1往期推荐Historical articles