تفاعل #66394

ord-40bdd2650dc84da68d73597eb7e292c0

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةheated the reaction mixture
  2. 2
    درجة الحرارةat reflux temp for 4 h
  3. 3
    استخلاصextracted with EtOAc
  4. 4
    غسيلThe combined extracts were washed with water, brine
  5. 5
    تجفيفdried over anhydrous Na2SO4
  6. 6
    ترشيحfiltered
  7. 7
    أخرىevaporated
  8. 8
    أخرىThe crude residue was purified by column chromatography

الإجراء التجريبي

A solution of tert-butyl(trans)-2-(4-bromophenyl)cyclopropylcarbamate (Intermediate F; 1 equiv), 1.2 equiv of the boronic acid, 3.0 equiv of K2CO3 in CH3CN+H2O (4:1) was degassed for 30 mins with Argon gas, added 0.01 equiv of Pd (PPh3)4, heated the reaction mixture at reflux temp for 4 h. The progress of the reaction was monitored by TLC, after completion, poured the reaction mixture into water, extracted with EtOAc. The combined extracts were washed with water, brine, dried over anhydrous Na2SO4, filtered and evaporated. The crude residue was purified by column chromatography to get tert-butyl(trans)-2-(1,1′-biphenyl-4-yl)cyclopropylcarbamate derivative

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08524717B2uspto-grants-2013_09