Reaktion #2186168

ord-0075226fa1d548c8a9e773e4d1c863d5

Reaktionsgleichung

CC(CCC(CO)C(C)CC(C)(C)C)CC(C)(C)C
2-(1,3,3-trimethyl-n-butyl)-5,7,7-trimethyl-n-octanol
O=P(Cl)(Cl)Cl
phosphorus oxychloride
CCN(CC)CC
triethylamine
CC(CCC(COP(=O)(Cl)Cl)C(C)CC(C)(C)C)CC(C)(C)C
[2-(1,3,3-trimethyl-n-butyl)-5,7,7-trimethyl-n-octyl] dichlorophosphate
Ausbeute 34.7%

Lösungsmittel

Reaktionsbedingungen

Temperatur
-10°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe mixture was reacted for 12 hours at 0 degrees C
  2. 2
    TemperaturThe mixture was then heated to 25 degrees C
  3. 3
    Sonstige, and a triethylamine hydrochloride was removed
  4. 4
    Filtrationby filtering

Vorschrift

With nitrogen substitution, 540 ml of toluene and 138.0 grams (0.9 moles) of phosphorus oxychloride were added and cooled to −10 degrees C. To this mixture, a solution of 243.5 grams (0.9 moles; 1.0 in molar ratio) of 2-(1,3,3-trimethyl-n-butyl)-5,7,7-trimethyl-n-octanol and 91.1 grams (0.9 moles) of triethylamine was dripped, and the mixture was reacted for 12 hours at 0 degrees C. The mixture was then heated to 25 degrees C., and a triethylamine hydrochloride was removed by filtering to obtain 1003.9 grams of a toluene solution of [2-(1,3,3-trimethyl-n-butyl)-5,7,7-trimethyl-n-octyl] dichlorophosphate (34.7% in concentration).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07569211B2uspto-grants-2009_08