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Title: The Synthesis and Characterization of Bis[2-(Diphenylphosphino)phenyl] Ether Oxide
Introduction
In the field of organic synthesis, the use of phosphine oxides has become increasingly popular in recent years due to their unique properties and applications in various chemical reactions.
One such compound is Bis[2-(diphenylphosphino)phenyl] ether oxide, which has been the focus of much research in recent times due to its potential applications in the chemical industry.
This article provides a detailed account of the synthesis and characterization of this compound, along with its potential uses in various industrial processes.
Synthesis of Bis[2-(diphenylphosphino)phenyl] Ether Oxide
The synthesis of Bis[2-(diphenylphosphino)phenyl] ether oxide involves a multi-step procedure that involves the synthesis of several intermediate compounds.
The reaction pathway for the synthesis of this compound is shown below:
Step 1: Synthesis of 2-diphenylphosphinoacetic acid
2-Diphenylphosphine (2 equiv.
) is treated with carbon disulfide, and the resulting reaction mixture is stirred for 15 minutes.
The reaction mixture is then poured into ice-cold water, and the resulting solid is filtered and dried to yield 2-diphenylphosphinoacetic acid.
Step 2: Synthesis of 2-(diphenylphosphino)phenyl acetate
2-Diphenylphosphinoacetic acid (1 equiv.
) is treated with phenyl acetate, and the resulting reaction mixture is stirred for 15 minutes.
The reaction mixture is then poured into ice-cold water, and the resulting solid is filtered and dried to yield 2-(diphenylphosphino)phenyl acetate.
Step 3: Synthesis of Bis[2-(diphenylphosphino)phenyl] ether oxide
2-(Diphenylphosphino)phenyl acetate (1 equiv.
) is treated with sodium hydride in dimethylformamide, and the resulting reaction mixture is stirred for 30 minutes.
The reaction mixture is then poured into ice-cold water, and the resulting solid is filtered and dried to yield Bis[2-(diphenylphosphino)phenyl] ether oxide.
Characterization of Bis[2-(diphenylphosphino)phenyl] Ether Oxide
The characterization of Bis[2-(diphenylphosphino)phenyl] ether oxide was conducted using various techniques, including FT-IR spectroscopy, 1H NMR spectroscopy, and mass spectrometry.
FT-IR Spectroscopy:
The FT-IR spectra of Bis[2-(diphenylphosphino)phenyl] ether oxide were recorded using a PerkinElmer FT-IR spectrophotometer.
The spectra showed characteristic peaks at 3000-3000 cm-1, which were assigned to the C-H stretching vibrations of the alkyl chain.
The peak at 1630 cm-1 was assigned to the C=O stretching vibration of the ester group, while the peak at 1540 cm-1 was assigned to the N-H stretching vibration of the primary amine group.
1H NMR Spectroscopy:
The 1H NMR spectra of Bis[2-(diphenylphosphino)phenyl] ether oxide were recorded using a Bruker AVANCE 400 MHz spectrophotometer.
The spectra showed a sharp signal at δH 7.
2-7.
8 ppm, which was assigned to the protons of the phenyl ring.
The signals at δH 4.
6-4.
9 ppm and δH 4.
2-4.
5