تفاعل #1447111

ord-8811a46e97394e3f8534247de4bc141b

معادلة التفاعل

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

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
-78°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.WAITthe resulting solution was left
  2. 2
    درجة الحرارةto warm to RT overnight
  3. 3
    ترشيحThe white slurry was filtered under an inert atmosphere
  4. 4
    أخرىall volatiles were removed

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07879815B2uspto-grants-2011_02