Diphenylphosphane chloride → (4-Methoxyphenyl)(diphenyl)phosphine

HRID 1967661Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1967661
[Cl-].[C:2]1([PH:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:15][O:16][C:17]1[CH:22]=[CH:21][C:20]([Mg]Br)=[CH:19][CH:18]=1>[NH4+].[Cl-]>[C:9]1([P:8]([C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[C:20]2[CH:21]=[CH:22][C:17]([O:16][CH3:15])=[CH:18][CH:19]=2)[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

Komponenten

4

Edukt 2

HCID 19695023Diphenylphosphane chlorideHCID 178491912HCID 178491912, Verbindung

Produkt 1

HCID 2775957(4-Methoxyphenyl)(diphenyl)phosphine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 25517Ammonium ChlorideLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

Diphenylphosphine chloride (5 mmol, 0.92 ml) was dissolved in TIM (25 ml). The solution was cooled to 0° C. 4-Methoxyphenyl magnesium bromide (6.5 mmol, 19 ml, 1.3 eq) was added dropwise to the solution over 20 minutes. The mixture was stirred for 3 hours. The mixture was allowed to warm to room temperature, and then stirred for another 5 hours after which saturated NH4Cl (20 ml) was added thereto to terminate the reaction. The inorganic salt was removed by suction filtration and the filtrate was extracted with dichloromethane (40 ml×3). The extract was dried over sodium sulfate and concentrated using an evaporator and an oil pump to give diphenyl-4-methoxyphenylphosphine.

Aufarbeitung

  1. temperatureto warm to room temperature
  2. additionwas added
  3. customto terminate
  4. customthe reaction
  5. customThe inorganic salt was removed by suction filtration
  6. extractionthe filtrate was extracted with dichloromethane (40 ml×3)
  7. dry with materialThe extract was dried over sodium sulfate
  8. concentrationconcentrated
  9. customan evaporator

Quellen und Nachweise

ORD-Eintrag
ord-2600a080cf17470d8f3c44d0dc20b535
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08420865B2

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