Реакция #1106666

ord-ac9cf472fe20486fb5e73b1f3619b2a4

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураwas refluxed for 18 h
  2. 2
    Экстракцияextracted with chloroform (2×200 mL)
  3. 3
    ПромывкаThe combined organic layer was washed with water, brine
  4. 4
    Сушкаdried over MgSO4
  5. 5
    Другоеevaporated to dryness
  6. 6
    ДругоеThe residue thus obtained
  7. 7
    Другоеwas purified by silica gel flash chromatography [CHCl3/MeOH/Et3N (44:5:1)]

Методика

A mixture of 1,5-dichloroanthraquinone (5.5 g, 20 mmol) and N,N,N′-trimethylethylenediamine (40 ml) was refluxed for 18 h. The mixture was cooled to room temperature, diluted with water (400 mL) and extracted with chloroform (2×200 mL). The combined organic layer was washed with water, brine, dried over MgSO4 and evaporated to dryness. The residue thus obtained was purified by silica gel flash chromatography [CHCl3/MeOH/Et3N (44:5:1)] to provide Compound 9. Abs (max, PBS pH 7.4)=508 nm. The structure of Compound 9 is given below:

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08715944B2uspto-grants-2014_05