Tributylamine → 2,2'-Bis((diphenylphosphaneyl)methyl)-1,1'-binaphthalene

HRID 1450015

Reaktionsgleichung

Reaktionsgleichung von HRID 1450015
[C:1]1([P:7]([CH2:15][C:16]2[CH:25]=[CH:24][C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[C:17]=2[C:26]2[C:35]3[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=3)[CH:29]=[CH:28][C:27]=2[CH2:36][P:37]([C:45]2[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=2)([C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=2)=O)([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(CCCC)CCCC)CCC.C1([SiH](Cl)Cl)C=CC=CC=1>C1(C)C(C)=CC=CC=1>[C:45]1([P:37]([CH2:36][C:27]2[CH:28]=[CH:29][C:30]3[C:35](=[CH:34][CH:33]=[CH:32][CH:31]=3)[C:26]=2[C:17]2[C:18]3[C:23](=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH:24]=[CH:25][C:16]=2[CH2:15][P:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)[C:39]2[CH:40]=[CH:41][CH:42]=[CH:43][CH:44]=2)[CH:46]=[CH:47][CH:48]=[CH:49][CH:50]=1

Komponenten

5

Edukt 3

HCID 7622TributylamineHCID 74207Dichloro(phenyl)silaneHCID 109525322,2'-Bis(diphenylphosphinylmethyl)-1,1'-binaphthyl

Produkt 1

HCID 109524072,2'-Bis((diphenylphosphaneyl)methyl)-1,1'-binaphthalene

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7237O-XyleneLösungsmittel

Versuchsvorschrift

20.48 g (0.03 mol) of 2,2'-bis(diphenylphosphinylmethyl)-1,1'-binaphthyl are suspended in 80 ml of xylene and 30.6 g (0.165 mol) of tri-n-butylamine in the absence of air and moisture, and 26.57 g (0.15 mol) of phenyldichlorosilane are added dropwise with stirring. The mixture is then refluxed for 13 hours to give a clear solution. Xylene is distilled off at atmospheric pressure, and the mixture is allowed to cool with stirring. This results in the formation of 2,2'-bis(diphenylphosphinomethyl)-1,1'-binaphthyl as a colorless solid, which is filtered off under an inert gas and washed with 20 ml of degassed acetone. 18.5 g (95%) of colorless crystals of melting point 160° to 161° C. are obtained.

Aufarbeitung

  1. temperatureThe mixture is then refluxed for 13 hours
  2. customto give a clear solution
  3. distillationXylene is distilled off at atmospheric pressure
  4. temperatureto cool
  5. stirringwith stirring

Quellen und Nachweise

ORD-Eintrag
ord-a987d8be2493433b91031fc849d6f300
Quelldatensatz
uspto-grants-1997_02
Patentnummer
US05600006

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