Bis(diphenylphosphino)methane → Bis(dicyclohexylphosphino)methane

HRID 260978Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 260978
[C:1]1([P:7]([CH2:14][P:15]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H][H]>C1CCCCC1>[CH:16]1([P:15]([CH2:14][P:7]([CH:8]2[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]2)[CH:1]2[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]2)[CH:22]2[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]2)[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1

Komponenten

4

Edukt 2

HCID 74952Bis(diphenylphosphino)methaneHCID 178418361HCID 178418361, Verbindung2×

Produkt 1

HCID 618458Bis(dicyclohexylphosphino)methane

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8078CyclohexaneLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A 300 ml. stainless steel high pressure reactor was charged, under a nitrogen atmosphere at atmospheric temperature, with a solution of ##STR1## hereinafter referred to as Nb(OC6H3Ph2 --2,6)2 (CH2C6H4 --4Me)3 (2.2 g., 2.5 mmol.) and bis(di-phenylphosphino)methane (25.0 g., 65.1 mmol.) in cyclohexane (55 ml.). The reactor was pressurized with hydrogen (1,200 psi) and heated at 100° C. for four days. During the course of the reaction the pressure dropped requiring the repressurization of the reactor four times. Thereupon, the reactor was cooled and the hydrogen gas vented. The cyclohexane was removed in vacuo and water (30 ml.) was added to the mixture. The mixture was extracted with diethyl ether (200 ml.) which extraction was repeated four times to yield a clear colorless solution. The ether was removed and the resultant solution was recrystallized from hot ethanol (120 ml.).

Aufarbeitung

  1. additionstainless steel high pressure reactor was charged, under a nitrogen atmosphere at atmospheric temperature, with a solution of ##STR1##
  2. customDuring the course of the reaction the pressure
  3. additiondropped
  4. temperatureThereupon, the reactor was cooled
  5. customThe cyclohexane was removed in vacuo and water (30 ml.)
  6. additionwas added to the mixture
  7. extractionThe mixture was extracted with diethyl ether (200 ml.) which extraction
  8. customto yield a clear colorless solution
  9. customThe ether was removed
  10. customthe resultant solution was recrystallized from hot ethanol (120 ml.)

Quellen und Nachweise

ORD-Eintrag
ord-ccba07ea3070499180d8ffa6f7394612
Quelldatensatz
uspto-grants-1996_06
Patentnummer
US05530162

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