Реакция #358209

ord-3f82b9299deb4e4aa0765f4c3fa12b68

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураheated to a boil
  2. 2
    Температураthe solution was heated
  3. 3
    Температураat reflux for 2 hours
  4. 4
    workup.ADDITIONThe reaction mixture was then poured onto ice
  5. 5
    Экстракцияthe aqueous phase was extracted with chloroform
  6. 6
    СушкаThe combined organic phases were dried over magnesium sulfate
  7. 7
    ДругоеThe purification

Методика

0.92 g (2.22 mmol) of 1-(2-tert. butylphenyl)-6-(2-hydroxyethyl)-1H-indolo[5,4,3-def]isoquinoline-2,5,7(6H)-trione was dissolved in 60 mL of chloroform and heated to a boil. Then, 15 mL (15.54 mmol) of phosphorus tribromide was added dropwise within 20 minutes and the solution was heated at reflux for 2 hours. The reaction mixture was then poured onto ice, and the aqueous phase was extracted with chloroform. The combined organic phases were dried over magnesium sulfate. The purification was carried out by column chromatography on silica gel with toluene as the developing solvent.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07452385B2uspto-grants-2008_11