Method for reducing thioamide compound

• Main Authors: YU YOUJIE, ZHU TONGQIN, ZHANG FENGLIAN
• Format: Patent
• Language: Chinese; English
• Published: 22.09.2017
• Subjects: ACYCLIC OR CARBOCYCLIC COMPOUNDS; ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAININGELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN,SULFUR, SELENIUM OR TELLURIUM; CHEMISTRY; HETEROCYCLIC COMPOUNDS; METALLURGY; ORGANIC CHEMISTRY

The invention provides a method for reducing a thioamide compound. The method comprises: at 80 DEG C and under nitrogen protection, taking thioamide as a substrate, adding ditert-butoxyazide (TBHN) and 4-dimethylamino pyridine borane complex (DMAP-BH3) as radical initiators, adding a catalytic amount of thiophenol, and performing stirring in acetonitrile for a proper time to obtain corresponding amine. The same conversion can be achieved by taking triethylborane/oxygen as an initiator at 25 DEG C. The reaction is non-toxic, and is mild in reaction condition, convenient to operate, good in function group tolerance, short in reaction time, and high in efficiency. 本发明提供了种还原硫代酰胺类化合的方法，在80℃以及氮气保护条件下，以硫代酰胺为底物，加入自由基引发剂二叔丁氧基叠氮(TBHN)，4-二甲氨基吡啶硼烷络合物(DMAP-BH)，以及催化量的苯硫酚，在乙腈中搅拌适当时间即可得到相应的胺。用三乙基硼/氧气做引发剂，25℃条件下，也能实现相同的转化。该反应具有无毒，反应条件温和，操作方便，官能团容忍性好，反应时间短，反应效率高等优点。