تفاعل #66119

ord-d92c74dec56243feb3f871ceca7d81c6

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةat reflux for 18 h
  3. 3
    درجة الحرارةThe mixture was cooled
  4. 4
    ترشيحthe inorganic salts filtered
  5. 5
    تركيزthe filtrate concentrated under vacuum
  6. 6
    أخرىto give a brown viscous liquid, which
  7. 7
    أخرىwas partitioned between dichloromethane and water
  8. 8
    أخرىThe organic phase was separated
  9. 9
    تركيزconcentrated in vacuo
  10. 10
    أخرىto obtain a residue which
  11. 11
    أخرىwas purified by column chromatography

الإجراء التجريبي

A mixture of p-nitro-phenol (6.0 g, 43.1 mmol), potassium carbonate (14.9 g, 108 mmol) and 1,2-dibromoethane (24.3 g, 129 mmol) in butanone (80 mL) was heated at reflux for 18 h. The mixture was cooled, the inorganic salts filtered and the filtrate concentrated under vacuum to give a brown viscous liquid, which was partitioned between dichloromethane and water. The organic phase was separated and concentrated in vacuo to obtain a residue which was purified by column chromatography using 4% ethyl acetate in petroleum ether as eluent to afford 1-(2-bromo-ethoxy)-4-nitro-benzene (7.5 g, 70%) as a light yellow solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08524705B2uspto-grants-2013_09