Reaktion #1539628

ord-8410bcace2c14a0594f00462ab0edfb3

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturit was heated to 120° C. over a period of 1 hour
  2. 2
    Sonstigereached 120° C.
  3. 3
    workup.WAITThe system was kept at a pressure of 2.67 kPa (20 mmHg) or lower for 3 hours
  4. 4
    Sonstigeto remove volatile matters

Vorschrift

Then, 207.6 g (2.0 mols) of trimethyl borate was added to 618 g (3.0 mols) of tripropylene glycol monomethyl ether. The mixture was heated to 60° C. with stirring in a dry nitrogen atmosphere. After the mixture was kept at 60° C. for 1 hour, it was heated to 120° C. over a period of 1 hour. After the temperature reached 120° C., the pressure in the system was gradually reduced. The system was kept at a pressure of 2.67 kPa (20 mmHg) or lower for 3 hours to remove volatile matters produced with progress of ester interchange reaction of boric acid and excess trimethyl borate, followed by filtration to obtain 610 g of a polymerizable boron-containing compound G (an esterification product of boric acid with tripropylene glycol monomethyl ether) represented by the formula (3). An infrared absorption spectrum of the resulting polymerizable boron-containing compound G was measured to confirm that the absorption band originating from hydroxyl group at 3300 cm−1 disappeared.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07473492B2uspto-grants-2009_01