تفاعل #60014

ord-eb6ad7a0b9d2406aad6f0d5931f4fdb6

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was heated
  2. 2
    درجة الحرارةto reflux for 24 hours under argon
  3. 3
    ترشيحfiltered
  4. 4
    أخرىAfter removal of solvent
  5. 5
    workup.DISTILLATIONby distillation
  6. 6
    أخرىthe product was purified

الإجراء التجريبي

4-Octylaniline (5.00 g, 244.4 mmol), 18-crown-6 (1.29 g, 4.9 mmol), K2CO3 (27.64 g, 194.8 mmol), 1-chloro-4-iodobenzene (14.51 g, 60.9 mmol, copper (6.19 g, 97.4 mmol), and 1,2-dichlorobenzene (100 mL) were added in a 250 mL flask with a condenser connected to a Dean Stark apparatus. The mixture was heated to reflux for 24 hours under argon. The reaction mixture was then cooled to room temperature, diluted with dichloromethane, and filtered. After removal of solvent by distillation, the product was purified using silica gel column chromatography using hexane as eluant. The yield was 4.18 g (40.3%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07425723B2uspto-grants-2008_09