반응 #1106666

ord-ac9cf472fe20486fb5e73b1f3619b2a4

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed for 18 h
  2. 2
    추출extracted with chloroform (2×200 mL)
  3. 3
    세척The combined organic layer was washed with water, brine
  4. 4
    건조dried over MgSO4
  5. 5
    기타evaporated to dryness
  6. 6
    기타The residue thus obtained
  7. 7
    기타was purified by silica gel flash chromatography [CHCl3/MeOH/Et3N (44:5:1)]

실험 절차

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:

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08715944B2uspto-grants-2014_05