Phosphorus trichloride → n-Butyl tert-butyl chlorophosphine

HRID 2360

Reaktionsgleichung

Reaktionsgleichung von HRID 2360
[P:1]([Cl:4])(Cl)Cl.[C:5]([Mg]Cl)([CH3:8])([CH3:7])[CH3:6].[CH2:11]([Mg]Cl)[CH2:12][CH2:13][CH3:14]>C(OCC)C>[CH2:11]([P:1]([C:5]([CH3:8])([CH3:7])[CH3:6])[Cl:4])[CH2:12][CH2:13][CH3:14]

Komponenten

5

Edukt 3

HCID 24387Phosphorus trichlorideHCID 178418265HCID 178418265, VerbindungHCID 178418310HCID 178418310, Verbindung

Produkt 1

HCID 12507378n-Butyl tert-butyl chlorophosphine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel2×

Reaktionsbedingungen

Temperatur
-25 °C

Versuchsvorschrift

To a solution of phosphorus trichloride (55 g) in dry diethyl ether (200 cm3) stirred and maintained at between -25° C. and -30° C. in an atmosphere of dry nitrogen a 2 molar solution of tert-butyl magnesium chloride in diethyl ether (200 cm3, solution supplied by Aldrich Chemical Co.) was added during 45 min. After a further 30 min., a 2 molar solution of n-butyl magnesium chloride (200 cm3, solution supplied by Aldrich Chemical Co.) was added in the same way. The suspension was stirred at -25° C. for a further 45 min., then allowed to reach ambient temperature, and finally boiled under reflux for 30 min., cooled, filtered to remove magnesium chloride, and distilled, yielding n-butyl tert-butyl chlorophosphine (30.8 g), b.p. 76°-78° C. under a pressure of 15 mm of mercury.

Aufarbeitung

  1. additionwas added during 45 min
  2. customto reach ambient temperature
  3. temperatureunder reflux for 30 min.
  4. temperaturecooled
  5. filtrationfiltered
  6. customto remove magnesium chloride
  7. distillationdistilled

Quellen und Nachweise

ORD-Eintrag
ord-e7d8772123ce4e13a0605b2c4b96576a
Quelldatensatz
uspto-grants-1998_03
Patentnummer
US05728853

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