反应 #75480

ord-f864972e90794ee39827fc1c7b384905

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.ADDITIONwas added
  2. 2
    温度The reaction mixture was refluxed under N2 for 22 h
  3. 3
    其他The solvent was evaporated
  4. 4
    洗涤The solid residue was washed with EtOH
  5. 5
    其他was dried under high vacuum

实验过程

To a mixture of 2,4-difluoroaniline (25 mmol, 3.2 g) in EtOH (10 mL) in an ice bath was added nitric acid (69% aq soln.; 1.8 mL) dropwise. After completion of the addition cyanamide (50% aq. soln.; 4 mL) was added. The reaction mixture was refluxed under N2 for 22 h. The solvent was evaporated. The solid residue was washed with EtOH and was dried under high vacuum to afford the title compound as a purple solid (2.32 g, 40%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06699854B2uspto-grants-2004_03