Phenylphosphonic acid dibutyl ester synthesis
- Product Name:Phenylphosphonic acid dibutyl ester
- CAS Number:1024-34-6
- Molecular formula:C14H23O3P
- Molecular Weight:270.3
Yield:1024-34-6 100 %Spectr.
Reaction Conditions:
with CuI(diethyl (1,10-phenanthrolin-4-yl)phosphonate)(triphenylphosphine)bromide;caesium carbonate in toluene; for 24 h;Inert atmosphere;Reflux;Reagent/catalyst;
Steps:
5 2.5. Cu(I)-catalyzed coupling of di-n-butyl phosphite with 4-iodoanisole
A Pyrex glass tube equipped with a Teflon stir bar, was charged with 4-iodoanisole (117 mg, 0.5 mmol), cesium carbonate (195 mg, 0.6 mmol) and Cu(Pphen)(PPh3)Br (1a-c, e) was sealed with rubber septum. The tube was evacuated and purged with N2 three times. Subsequently, toluene (2 ml) and di-n-butyl phosphite (233 μl, 1.2 mmol) were added through a syringe into the tube. The reaction mixture was stirred at reflux and periodically analyzed using 1H NMR spectroscopy.
References:
Mitrofanov, A.Yu.;Bessmertnykh-Lemeune;Beletskaya [Inorganica Chimica Acta,2015,vol. 431,p. 297 - 301]
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