Reaktion #352902

ord-f1a8535af413410c83dc3b564b346c4e

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeA 3-neck, 250-mL round bottom flask equipped with a reflux condenser
  2. 2
    workup.STIRRINGThe reaction mixture was kept stirred for an additional 30 minutes
  3. 3
    FiltrationThe solution was filtered
  4. 4
    Sonstigeevaporated to dryness
  5. 5
    Sonstigeto recover the product

Vorschrift

A 3-neck, 250-mL round bottom flask equipped with a reflux condenser was charged with isocyanatoethyl methacrylate (7.79 g), 1,1'-bi-2-naphthol (1.3 mg) and 50 mL of methylene chloride. While stirring, cyclohexylamine (5.24 g) and dibutyltin dilaurate (52.3 mg) in 50 mL of methylene chloride were added over a 15 minute period. The reaction mixture was kept stirred for an additional 30 minutes. The solution was filtered and evaporated to dryness to recover the product. The product was characterized by H-NMR, 0.72-2.10 ppm (m, 1H), 1.90 ppm (s, 3H), 3.45 ppm (t, 2H), 3.50 ppm (hidden, 1H), 4.18 ppm (t, 2H), 5.12 ppm (s, 1H), 5.26 ppm (s, 1H), 5.52 ppm (s, 1H), 6.10 ppm (s, 1H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05648515uspto-grants-1997_07