تفاعل #60420

ord-a20d3aba619c4acdb6c3b52ebe061293

المذيبات

ظروف التفاعل

درجة الحرارة
90°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحThe reaction mixture was passed through Celite for filtration
  2. 2
    workup.ADDITIONbrine was added to the filtrate
  3. 3
    استخلاصthe mixture was extracted with ethyl acetate
  4. 4
    تجفيفThe organic layer was dried over anhydrous magnesium sulfate
  5. 5
    ترشيحthe desiccant was filtered off
  6. 6
    تركيزthe filtrate was concentrated under reduced pressure

الإجراء التجريبي

To a solution of 1-(4,4-diethylcyclohex-1-enyl)-4-methoxy-2-nitrobenzene (2.4 g, 8.3 mmol) prepared in Example (6d) in ethanol (20 mL) were added an aqueous solution (5 mL) of ammonium chloride (2.2 g, 41 mmol) and iron powder (1.2 g, 20.7 mmol), and the mixture was stirred at an external temperature of 90° C. for 1 hour. The reaction mixture was passed through Celite for filtration, and then brine was added to the filtrate and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, the desiccant was filtered off, and then the filtrate was concentrated under reduced pressure to give 2.6 g of the title compound as a yellow oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07425554B2uspto-grants-2008_09