Phosphorus trichloride → Diisopropylphosphoramidous dichloride

HRID 83974

Reaktionsgleichung

Reaktionsgleichung von HRID 83974
C(N([P:8]([N:10]([CH:14]([CH3:16])[CH3:15])[CH:11]([CH3:13])[CH3:12])[Cl:9])C(C)C)(C)C.P(Cl)(Cl)[Cl:18]>C(#N)C>[CH:11]([N:10]([P:8]([Cl:18])[Cl:9])[CH:14]([CH3:16])[CH3:15])([CH3:13])[CH3:12]

Komponenten

4

Edukt 2

HCID 24387Phosphorus trichlorideHCID 2733425Bis(diisopropylamino)chlorophosphine

Produkt 1

HCID 5139911Diisopropylphosphoramidous dichlorideAusbeute 81 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

Bis-(N,N-Diisopropylamino)chlorophosphine, 10 grams (37 mmols), was dissolved in 500 ml of anhydrous acetonitrile. Phosphorus trichloride, 5.16 grams (37 mmols), was added to the solution and the reaction was allowed to stir over-night at room temperature. The reaction was assayed for completion by 31P NMR of an aliquot of the reaction using an external lock. Complete conversion of the starting material at δ 134 ppm to the product at δ 165 ppm was observed. The solvent was evaporated from the reaction mixture on a rotary evaporator and the resulting oil distilled under vacuum yielding 5.7 grams of product (81% yield).

Aufarbeitung

  1. customThe solvent was evaporated from the reaction mixture on a rotary evaporator
  2. distillationthe resulting oil distilled under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-5b434021ae2847e99833fbda32072bfd
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08846898B2

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