Reaktion #358811

ord-9f2dbb30cce642bf844fae54bdac4633

Reaktionsbedingungen

Temperatur
65°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeequipped with a condenser
  2. 2
    Sonstigemechanical mixer, thermometer, nitrogen purge
  3. 3
    workup.ADDITIONA single drop of dibutyltin dilaurate was added and within 5 hours the reaction
  4. 4
    SonstigeThe product was then removed from the flask as a colorless liquid with a viscosity of 21,000 cPs

Vorschrift

3-Methyl-3-oxetane methanol (20.00 g, 0.1958 mole) and m-TMI (39.49 g, 0.1958 mole) were combined in a 250-ml four-neck round bottom flask equipped with a condenser, mechanical mixer, thermometer, nitrogen purge and oil bath. The reaction was placed under nitrogen with stirring and heated to 65° C. in the oil bath. A single drop of dibutyltin dilaurate was added and within 5 hours the reaction was complete based on depletion of the FT-IR isocyanate peak (2254 cm−1). The product was then removed from the flask as a colorless liquid with a viscosity of 21,000 cPs.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07452943B2uspto-grants-2008_11