تفاعل #75480

ord-f864972e90794ee39827fc1c7b384905

معادلة التفاعل

Nc1ccc(F)cc1F
2,4-difluoroaniline
O=[N+]([O-])O
nitric acid
N#CN
cyanamide
N=C(N)Nc1ccc(F)cc1F.O=[N+]([O-])O
title compound
المردود 40.0%
N=C(N)Nc1ccc(F)cc1F.O=[N+]([O-])O
N-(2,4-Difluoro-phenyl)-guanidine nitrate
المردود 40.0%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added
  2. 2
    درجة الحرارةThe reaction mixture was refluxed under N2 for 22 h
  3. 3
    أخرىThe solvent was evaporated
  4. 4
    غسيلThe solid residue was washed with EtOH
  5. 5
    أخرىwas dried under high vacuum

الإجراء التجريبي

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%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06699854B2uspto-grants-2004_03