Reaction #684941

ord-091c74c35b4a4bfb922d1afbbb81ec01

Reaction equation

CCO
ethanol
ClP(Cl)Cl
phosphorous trichloride
CC(C)NC(C)C
diisopropylamine
CC(C)N(PN(C(C)C)C(C)C)C(C)C
bis(diisopropylamino)phosphine
→
CC(C)N(C(C)C)P(Cl)N(C(C)C)C(C)C
Bis(diisopropylamino)chlorophosphine

Reactants

CCO
ethanol
ClP(Cl)Cl
phosphorous trichloride
CC(C)NC(C)C
diisopropylamine
CC(C)N(PN(C(C)C)C(C)C)C(C)C
bis(diisopropylamino)phosphine

Reagents

None

Solvents

Cc1ccccc1
toluene

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    workup.WAITto proceed for several days
  2. 2
    FiltrationAfter filtering the mixture
  3. 3
    Otherremoving the solvent

Procedure

Bis(diisopropylamino)chlorophosphine was synthesized by reacting phosphorous trichloride and diisopropylamine in toluene. Fifty ml of the resulting bis(diisopropylamino)phosphine was placed in a 250 ml flask and 3.01 ml of ethanol added slowly over a two minute period and the reaction allowed to proceed for several days. After filtering the mixture and removing the solvent, the structure of the bis(diisopropylamino)ethylphosphite ester reagent was analyzed by 31P and 1H NMR (31P NMR in CD3CN 125.9 ppm).

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07897338B2uspto-grants-2011_03