تفاعل #167034

ord-a82ef3c06d9e4a16872ba8ff2dba8161

المذيبات

ظروف التفاعل

درجة الحرارة
25°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصThe mixture was extracted with EtOAc (2×)
  2. 2
    غسيلThe combined organic phase was washed with water and brine
  3. 3
    تجفيفdried with Na2SO4
  4. 4
    تركيزConcentration under reduced pressure
  5. 5
    أخرىgave pale solid
  6. 6
    أخرىThe re-crystallization from CH3CN/MeOH

الإجراء التجريبي

To the solution of 4,4′-dibromo-2,2′-dinitro-biphenyl (6.58 g, 16.5 mmol) in DMF (50 ml) at 0° C. was added a solution of sodium methoxide in Methanol (4.4 M, 4.5 ml, 19.8 mmol). The mixture was stirred at 25° C. for 12 hours and was poured into ice-water (140 ml). The mixture was extracted with EtOAc (2×). The combined organic phase was washed with water and brine and dried with Na2SO4. Concentration under reduced pressure gave pale solid. The re-crystallization from CH3CN/MeOH gave 4,4′-dibromo-2-methoxy-2′-nitro-biphenyl as a white solid (3.76 g).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08841278B2uspto-grants-2014_09