반응 #1447111

ord-8811a46e97394e3f8534247de4bc141b

반응 방정식

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

용매

반응 조건

온도
-78°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07879815B2uspto-grants-2011_02