反应 #214841

ord-01a85a6c040c4d478281a98218ad40d8

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩The mixture is concentrated
  2. 2
    workup.STIRRINGstirred with water
  3. 3
    萃取extracted with dichloromethane
  4. 4
    干燥The resulting dichloromethane solution is dried
  5. 5
    其他evaporated

实验过程

12.55 parts by weight of butylmercaptan is dripped into a suspension of 3.33 parts by weight of sodium hydride in 180 parts by weight of tetrahydrofuran. A solution of 27.5 parts by weight of 1-[2-chloro-2-(2,4-dichlorophenyl)-ethyl]-1,2,4-triazole in 50 parts of tetrahydrofuran is then dripped in and the mixture is stirred for 3 days at room temperature. The mixture is concentrated, stirred with water, and extracted with dichloromethane. The resulting dichloromethane solution is dried and evaporated. There is obtained 29.5 parts of crude 1-[2-n-butylmercapto-2-(2,4-dichlorophenyl)-ethyl]-1,2,4-triazole, which is dissolved in ethyl acetate. When hydrogen chloride is passed into the ethyl acetate solution, 25.9 parts of 1-[2-n-butylmercapto-2-(2,4-dichlorophenyl)-ethyl]-1,2,4-triazole hydrochloride, m.p. 143° C., precipitates out.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04256754uspto-grants-1981_03