تفاعل #84864

ord-1523efd715ef4d52956632cd0dafdea7

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصThe mixture was extracted with EtOAc the combined
  2. 2
    غسيلorganics were washed with saturated aqueous NaHCO3 and brine
  3. 3
    تجفيفthen dried over Na2SO4
  4. 4
    تركيزconcentrated in vacuo
  5. 5
    أخرىPurification by chromatography (10-20% EtOAc-hexanes)

الإجراء التجريبي

To a solution of 1-(4-bromo-3,5-dimethoxyphenyl)propan-1-one (1.50 g, 5.49 mmol) in anhydrous THF (20 mL) was added pyridinium tribromide (1.93 g, 6.04 mmole). The reaction was stirred at room temperature for 2 hrs then neutralized with a solution of saturated aqueous NaHCO3. The mixture was extracted with EtOAc the combined organics were washed with saturated aqueous NaHCO3 and brine then dried over Na2SO4 and concentrated in vacuo. Purification by chromatography (10-20% EtOAc-hexanes) gave 2-bromo-1-(4-bromo-3,5-dimethoxyphenyl)propan-1-one as an orange oil (1.09 g, 56% yield).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09434707B2uspto-grants-2016_09