期刊文献+

对三氟甲基苯硫酰胺的合成

Synthesis of p-(Trifluoromethyl)thiobenzamide
下载PDF
导出
摘要 三氟甲基氯苯与氰化钾在经还原性金属粉末还原生成的三(三苯基膦)合镍(0)催化下反应得到三氟甲基苯甲腈,再与H2S发生加成反应,生成对三氟甲基苯硫酰胺。试验了各种条件对反应的影响,产品收率达90%,纯度达97%,并经IR和GC-MS检测,结构正确。工艺操作简单、反应条件温和。 p-trifluoromethylbenzonitrile was prepared from p-(trifluoromethyl)chlorobenzene and potussium cyanide catalyzed by tris(triphenylphosphine)nickle(0), which was prepared from anhydrous NiCl2 and triphenylphosphine in the presence of zinc.And then, the produced intermideate, p-trifluoromethylbenzonitrile was treated with hydrogen sulfide to give p-(trifluoromethyl)thiobenzamide and the yield of 90% with the purity of 99.7% was obtained for the objective product.The structure is correct through IR and GC-MS testing.The operation process is simple and reaction condition is moderate.
出处 《化工生产与技术》 CAS 2009年第1期1-4,共4页 Chemical Production and Technology
基金 国家科技支撑计划课题(2007BAI34B07) 国家自然科学基金项目(20776127) 浙江省科技计划项目(2008C01006-1)
关键词 对三氟甲基苯硫酰胺 对三氟甲基氯苯 三(三苯基膦)合镍(0) 对三氟甲基苯甲腈 合成 p-(trifluoromethyl)thiobenzamide p-(trifluoromethyl)chlorobenzene tris(triphenylphosphine)nickle(0) p-trifluoromethylbenzonitrile synthesis
  • 相关文献

参考文献7

  • 1Banker P, Cadilla R, Lambert M, et al. Preparation of thiazole and oxazole derivatives as activators of human peroxisome proliferator activated receptors: WO, 2002059098[P], 2002- 08-01. 被引量:1
  • 2You Q D, Zhou H Y, Wang Q Z, et al. Preparation of N-unsubstituted thioamides by a modified Willgerodt-Kindler reaction [J]. Org Prep Proced Int, 1991, 23(4): 435-438. 被引量:1
  • 3Jian FF, Zhao PS, Zhang L, et al. Synthesis, structure and quantum chemical calculations on p-trifluoromethylphenyl thioacid amide [J]. J Fluorine Chem, 2006, 127(1): 63-67. 被引量:1
  • 4Sakakibara Y, Okuda F, Shimobayashi A, et al. The cyanation of aromatic halides catalyzed by nickel(0) complexes generated in situ. I. General scope and limitations [J]. Bull Chem Soc Jpn, 1988, 61(6): 1 985-1 990. 被引量:1
  • 5Cassar L, Foa M, Montanari F, et al. Phase-transfer catalysis in the nickel-catalyzed cyanation of aryl halides [J]. J Org Chem, 1979, 173(3): 335-339. 被引量:1
  • 6Cristau H J, Ouali A, Spindler J F, et al. Mild and efficient copper-catalyzed cyanation of aryl iodides and bromides [J]. Chem Eur J, 2005, 11(8): 2 483-2 492. 被引量:1
  • 7Colon I, Kelsey D R. Coupling of aryl chlorides by nickel and reducing metals [J], J Org Chem, 1986, 51(14): 2 627- 2 637. 被引量:1

相关作者

内容加载中请稍等...

相关机构

内容加载中请稍等...

相关主题

内容加载中请稍等...

浏览历史

内容加载中请稍等...
;
使用帮助 返回顶部