تفاعل #4862

ord-adb591f5d8e14cf994f271977a5de703

المذيبات

ظروف التفاعل

درجة الحرارة
100°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe aqueous layer was separated
  2. 2
    غسيلthe organic washed twice with 100 ml portions of 2N HCl
  3. 3
    ترشيحAfter filtering the organic phase
  4. 4
    غسيلwashing with saturated KHCO3 and brine
  5. 5
    تجفيفdrying over MgSO4, it
  6. 6
    تركيزwas concentrated on the steam bath
  7. 7
    أخرىThe resulting solid product was purified by flash chromotography

الإجراء التجريبي

A mixture 9.3 g (50 mmole) of 2-bromo-m-xylene, 15.0 g (80 mmole) of N-allylphthalimide, 0.56 (2.5 mmole) of paladium acetate and 1.44 (5.5 mmole) of triphenylphosphine were dissolved in 111 ml of triethylamine. The solution was placed in a sealed container and heated at 100° C. for 24 hours. The reaction was then diluted with 800 ml of ether and 200 ml of water. The aqueous layer was separated and the organic washed twice with 100 ml portions of 2N HCl. After filtering the organic phase, washing with saturated KHCO3 and brine, and drying over MgSO4, it was concentrated on the steam bath. The resulting solid product was purified by flash chromotography and used in subsequent reactions.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04727189uspto-grants-1988_02