Reaktion #1358515

ord-442edf14060c419090fecadc82050932

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Waschenwashed with H2O (3×30 mL)
  2. 2
    Trocknenthen dried (Na2SO4)
  3. 3
    Filtrationfiltered
  4. 4
    Einengenconcentrated to an oil
  5. 5
    Filtrationfilter column
  6. 6
    Sonstigeto remove baseline impurities

Vorschrift

4,5-Dinitro-10-aza-tricyclo[6.3.1.02,7]dodeca-2(7),3,5-triene-10-carboxylic acid tert-butyl ester (500 mg, 1.43 mmol) and 1-butylamine (1.42 mL, 14.3 mmol) were combined in THF (5 mL) and stirred 4 hours. The mixture was diluted with ethyl acetate (50 mL) and washed with H2O (3×30 mL) then dried (Na2SO4), filtered and concentrated to an oil. This oil was passed through a Silica gel filter column to remove baseline impurities eluting with 30% ethyl acetate/hexanes (510 mg, 1.41 mmol, 99%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07205300B2uspto-grants-2007_04