تفاعل #60124

ord-680c55eea424449eb93b061849d47654

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرى0.5 ml water and purged with nitrogen
  2. 2
    تركيزThe reaction mixture was concentrated in vacuo
  3. 3
    workup.ADDITIONdiluted with water and ethyl acetate
  4. 4
    استخلاصThe solution was extracted three times with ethyl acetate
  5. 5
    تجفيفdried over sodium sulfate
  6. 6
    أخرىpurified by column chromatography
  7. 7
    غسيلeluting with 10% ethylacetate 90% hexanes

الإجراء التجريبي

1 mmol 2,6-dichloro-3-nitropyridine, 1.05 mmol of 2,4-dichlorobenzeneboronic acid, and 3 mmol of Na2CO3, were dissolved in 1.5 ml THF and 0.5 ml water and purged with nitrogen. 0.05 mmol of [1,1′-Bis(diphenylphosphino)-ferrocene]dichloro-palladium(II) was added to reaction and stirred at room temperature under nitrogen for fourteen hours. The reaction mixture was concentrated in vacuo and diluted with water and ethyl acetate. The solution was extracted three times with ethyl acetate, dried over sodium sulfate, and purified by column chromatography eluting with 10% ethylacetate 90% hexanes to obtain 2-(2,4-dichlorophenyl)-6-chloro-3-nitropyridine.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07425557B2uspto-grants-2008_09