Reaktion #712388

Reaktionsgleichung

oleylamine

oleic acid

trioctylphosphine oxide

selenium

diphenyl ether

trioctylphosphine

selenium

→

di-n-octylphosphinic acid

Lösungsmittel

methanol

toluene

acetonitrile

1-octadecene

1-octadecene

1-methyl-2-pyrrolidinone

NMP

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstige0.1M Se-ODE was prepared
2. 2
   Sonstigetrioctylphosphine oxide (TOPO) was recrystallized from acetonitrile
3. 3
   Sonstigewas prepared in advance

Vorschrift

Materials. 1-methyl-2-pyrrolidinone (99.5%, Aldrich), 1-octadecene (90%, Aldrich), acetonitrile (99.9%, Fisher Chemical), BiCl3 (99.999%, Strem), CdO (99.5%, Aldrich), diphenyl ether (99%, Aldrich), methanol (ACS grade, VWR), oleic acid (90%, Aldrich), oleylamine (70% Aldrich), selenium (99.99%, Strem), trioctylphosphine (90%, Aldrich), trioctylphosphine oxide (99%, Strem), toluene (ACS grade, VWR). 0.1M Se-ODE was prepared by dissolving selenium powder in 1-octadecene at 180° C. for 5 hr under inert atmosphere according to the procedure by Bullen et al.[42]; trioctylphosphine oxide (TOPO) was recrystallized from acetonitrile prior to use; di-n-octylphosphinic acid (DOPA) was synthesized according to the procedure reported by Wang et al.[1]; a stock suspension of 2 mM BiCl3 in NMP was prepared in advance.

Quelle