Reaktion #687344

ord-8d031b47dd414a35bbbbe73625e0193b

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionto extract
  2. 2
    WaschenThe organic layer was washed twice with 50 ml of water
  3. 3
    Trocknendried by magnesium sulfate
  4. 4
    Einengenconcentrated by evaporation
  5. 5
    SonstigeThe organic layer was purified by silica gel column chromatography
  6. 6
    Sonstigevacuum dried under a temperature of 70° C.

Vorschrift

A mixed solution of 1.5 g of the above-mentioned 1,3,6-tri(4-methylphenyl)pyrene, 0.68 g of N-bromosuccinimide and 30 ml of dimethylformamide was stirred under nitrogen gas stream at a temperature of 60° C. for 6 hours. After cooling the mixed solution to room temperature, 50 ml of water was injected thereinto to extract therefrom with 100 ml of dichloromethane. The organic layer was washed twice with 50 ml of water, dried by magnesium sulfate and thereafter concentrated by evaporation. The organic layer was purified by silica gel column chromatography and thereafter vacuum dried under a temperature of 70° C. to obtain 1.5 g of 1-bromo-3,6,8-tri(4-methylphenyl)pyrene as pale-yellow powder.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07901794B2uspto-grants-2011_03