Reaktion #1447111

ord-8811a46e97394e3f8534247de4bc141b

Reaktionsgleichung

CCN(CC)CC
Et3N
Oc1cccc2ccccc12
1-naphthol
O=P(Cl)(Cl)Cl
phosphorus oxychloride
O=P(Cl)(Cl)Oc1cccc2ccccc12
title compound
O=P(Cl)(Cl)Oc1cccc2ccccc12
1-Naphthyl dichlorophosphate

Lösungsmittel

Reaktionsbedingungen

Temperatur
-78°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.WAITthe resulting solution was left
  2. 2
    Temperaturto warm to RT overnight
  3. 3
    FiltrationThe white slurry was filtered under an inert atmosphere
  4. 4
    Sonstigeall volatiles were removed

Vorschrift

To 1-naphthol in Et2O (0.23 M) was added phosphorus oxychloride (1.0 eq.) and the solution was cooled to −78° C. Neat Et3N (1.0 eq) was added and the resulting solution was left to warm to RT overnight. The white slurry was filtered under an inert atmosphere and all volatiles were removed to yield the title compound as a colorless liquid that was used without further purification in the next step. 31P NMR (400 MHz, CDCl3): δ 3.93 ppm.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07879815B2uspto-grants-2011_02