Sodium Iodide → Dimethyl acetyl phosphate

HRID 1741762Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1741762
[P:1]([O-:7])([O:5][CH3:6])([O:3][CH3:4])=[O:2].[Na+].P(OC)(OC)(OC)=O.[I-].[Na+].[C:19](Cl)(=[O:21])[CH3:20]>O1CCCC1>[P:1]([O:7][C:19](=[O:21])[CH3:20])([O:5][CH3:6])([O:3][CH3:4])=[O:2]

Komponenten

6

Edukt 4

HCID 5238Sodium IodideHCID 6367Acetyl chlorideHCID 10541Trimethyl PhosphateHCID 23663684Sodium dimethyl phosphate

Produkt 1

HCID 14665382Dimethyl acetyl phosphateAusbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A suspension of sodium dimethyl phosphate (14.8 g, 0.1 mmol, from trimethyl phosphate and sodium iodide and acetyl chloride (7.8 g, 0.1 mmol) in dry tetrahydrofuran (80 mn) was stirred for two days at room temperature in a flask fitted with a drying tube. The reaction solution was filtered and the tetrahydrofuran was removed under reduced pressure. The resulting colorless liquid was Kugelrohr-distilled (Aldrich Kugelrohr apparatus, 55°-60° C. 0.30 torr) to give 14.2 g (80%) of dimethyl acetyl phosphate.

Aufarbeitung

  1. customfitted with a drying tube
  2. filtrationThe reaction solution was filtered
  3. customthe tetrahydrofuran was removed under reduced pressure
  4. distillationThe resulting colorless liquid was Kugelrohr-distilled (Aldrich Kugelrohr apparatus, 55°-60° C. 0.30 torr)

Quellen und Nachweise

ORD-Eintrag
ord-066fbcfb554c4382980d8c292f3fdf83
Quelldatensatz
uspto-grants-1994_08
Patentnummer
US05334707

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