تفاعل #70290

ord-7ee7410d972e4921b333c9256dc0a28a

الكواشف

المذيبات

ظروف التفاعل

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

المعالجة

  1. 1
    ترشيحThe crude was filtered through Celite
  2. 2
    غسيلwashed with ethanol
  3. 3
    أخرىThe solvent was evaporated
  4. 4
    workup.ADDITIONethyl acetate was added
  5. 5
    غسيلwas washed with NaHCO3 4% aqueous solution, water and brine
  6. 6
    أخرىThe crude was purified by chromatography
  7. 7
    غسيلeluting with DCM/MeOH

الإجراء التجريبي

To a solution of 2-(benzyloxy)-5-nitro-3-phenylpyridine (0.98 mmol, 0.3 g) in 10 mL of ethanol, 0.1 mL of HCl 35% and 0.27 g of Fe was added. The mixture was heated at 90° C. for 4 hours. The crude was filtered through Celite and washed with ethanol. The solvent was evaporated, ethyl acetate was added and was washed with NaHCO3 4% aqueous solution, water and brine. The crude was purified by chromatography eluting with DCM/MeOH mixtures affording 0.22 g (yield 79%) of expected product.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08536165B2uspto-grants-2013_09