Reaktion #8442

ord-32bf5b9791c7448ca1a7e797c6eb1088

Reaktionsgleichung

CC(=O)OC(C)=O
acetic anhydride
CCN(CC)CC
triethylamine
CN(C)c1ccccn1
dimethylaminopyridine
OCCOc1ccc(-c2nnnc(-c3cccc4ccccc34)c2-c2cccc3ccccc23)c(O)c1
product
OCCOc1ccc(-c2nnnc(-c3cccc4ccccc34)c2-c2cccc3ccccc23)c(O)c1
bis-α-naphthyl-(4-[2-hydroxy-ethoxy]-2-hydroxy-phenyl)-triazine
CC(=O)OCCOc1ccc(-c2nnnc(-c3cccc4ccccc34)c2-c2cccc3ccccc23)c(O)c1
bis-αnaphthyl-(4-[2-acetoxy-ethoxy]-2-hydroxy-phenyl)-triazine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture is heated to boiling
  2. 2
    Sonstigethe solvent is removed in vac
  3. 3
    WaschenThe organic phase is washed with water
  4. 4
    Trocknendried with magnesium sulfate
  5. 5
    SonstigeAfter removal of the solvent
  6. 6
    Sonstigethe residue is chromatographed on silica gel
  7. 7
    Sonstigeyielding the product

Vorschrift

9.11 g of acetic anhydride, 18.1 g of triethylamine and 0.73 g of dimethylaminopyridine in 400 ml of anhydrous dichloromethane are added to the product from Example A9. The reaction mixture is heated to boiling. When the reaction is complete (monitoring by TLC), the solvent is removed in vac. and the residue is taken up in dichloromethane. The organic phase is washed with water and dried with magnesium sulfate. After removal of the solvent, the residue is chromatographed on silica gel, yielding the product having the following NMR data:

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07087753B2uspto-grants-2006_08