تفاعل #60236

ord-aff8d328fb5246128c3497ee689c6469

معادلة التفاعل

CNCCNC
N,N′-dimethylethylenediamine
c1ccc(Nc2ccccc2)cc1
diphenylamine
Brc1ccc(I)cc1
4-bromoiodobenzene
Brc1ccc(N(c2ccccc2)c2ccccc2)cc1
white crystal
المردود 70.2%
Brc1ccc(N(c2ccccc2)c2ccccc2)cc1
4-bromotriphenylamine
المردود 70.2%

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةrefluxed for 24 hours under argon atmosphere
  2. 2
    ترشيحthe mixture was filtered
  3. 3
    أخرىto remove an insoluble matter
  4. 4
    تركيزthe filtrate was concentrated

الإجراء التجريبي

N,N′-dimethylethylenediamine 1.76 g was added to diphenylamine 16.9 g, 4-bromoiodobenzene 28.2 g sodium t-butoxide 14.4 g, copper powder 3.81 g and a xylene 100 ml solution, and the mixture was heated and refluxed for 24 hours under argon atmosphere. After cooled down to room temperature, the mixture was filtered to remove an insoluble matter, and the filtrate was concentrated. The residue was refined by silica gel chromatography to obtain 22.7 g of white crystal of 4-bromotriphenylamine.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07425654B2uspto-grants-2008_09