反应 #63135

ord-ab6b7f94f8af400198e19d6319e1a668

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他after which it is evaporated down in vacuo
  2. 2
    洗涤the solution is washed in succession with saturated sodium bicarbonate solution and saturated sodium chloride solution
  3. 3
    干燥The organic phase is dried over magnesium sulphate

实验过程

1.2 ml (0.0129 mol) of acetic anhydride and 0.6 ml (0.0143 mol) of 98% strength nitric acid are added in succession to 5 g (0.0113 mol) of 5-dichloroacetamido-1-(2,3,6-trichloro-4-trifluoromethyl-phenyl)-pyrazole in 10 ml of glacial acetic acid at room temperature. The mixture is stirred for 20 hours, after which it is evaporated down in vacuo, the residue is taken up in 50 ml of dichloromethane and the solution is washed in succession with saturated sodium bicarbonate solution and saturated sodium chloride solution. The organic phase is dried over magnesium sulphate and freed from the solvent in vacuo. 4.2 g (76.4% of theory) of 5-dichloroacetamido-4-nitro-1-(2,3,6-trichloro-4-trifluoromethyl-phenyl)-pyrazole of melting point 112° C.-120° C. are obtained.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04764202uspto-grants-1988_08