Tert‐butyl chloride was synthesised at the Deuteration Facility at ISIS Neutron and Muon Source, STFC Rutherford Appleton Laboratory in Oxfordshire, UK. Phosphorus trichloride (99%), magnesium ribbon (>99.5%), copper(I) iodide (>99.5%) and lithium bromide (>99%) were purchased from Sigma Aldrich and used as received. The glovebox used in this work was MBraun Labmaster dp, operating typically under argon, at or below 0.6 ppm of H2O and O2. 13C and 31P NMR spectra were recorded on a Bruker Avance DPX 400 MHz spectrometer. Electrospray mass spectrometry measurements were performed using a Waters LCT Premier mass spectrometer.
Phosphorus trichloride
Manufactured by Merck Group
Phosphorus trichloride is an inorganic compound with the chemical formula PCl3. It is a colorless, fuming liquid with a pungent odor. Phosphorus trichloride is primarily used as an intermediate in the production of other phosphorus-containing compounds.
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2 protocols using phosphorus trichloride
1
Synthesis and Characterization of tert-Butyl Chloride
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Tert‐butyl chloride was synthesised at the Deuteration Facility at ISIS Neutron and Muon Source, STFC Rutherford Appleton Laboratory in Oxfordshire, UK. Phosphorus trichloride (99%), magnesium ribbon (>99.5%), copper(I) iodide (>99.5%) and lithium bromide (>99%) were purchased from Sigma Aldrich and used as received. The glovebox used in this work was MBraun Labmaster dp, operating typically under argon, at or below 0.6 ppm of H2O and O2. 13C and 31P NMR spectra were recorded on a Bruker Avance DPX 400 MHz spectrometer. Electrospray mass spectrometry measurements were performed using a Waters LCT Premier mass spectrometer.
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Tert‐butyl chloride was synthesised at the Deuteration Facility at ISIS Neutron and Muon Source, STFC Rutherford Appleton Laboratory in Oxfordshire, UK. Phosphorus trichloride (99%), magnesium ribbon (>99.5%), copper(I) iodide (>99.5%) and lithium bromide (>99%) were purchased from Sigma Aldrich and used as received. The glovebox used in this work was MBraun Labmaster dp, operating typically under argon, at or below 0.6 ppm of H2O and O2. 13C and 31P NMR spectra were recorded on a Bruker Avance DPX 400 MHz spectrometer. Electrospray mass spectrometry measurements were performed using a Waters LCT Premier mass spectrometer.
2
Drying and Purification of Ionic Liquids
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For the NMR and Raman experiments, the ILs 1-hexyl-3-methylimidazolium chloride (IoLiTec, 99 %), 1-hexyl-3-methylimidazolium bromide (IoLiTec, 99 %) and 1-hexyl-3methylimidazolium bis(trifluoromethylsulfonyl)imide (IoLiTec, 99 %) were dried at 110
• C for 12 h under vacuum. To remove even traces of water for the synchrotron experiments, the ILs were dried at 70 • C for 24 h, at 110 • C for 12 h and finally at 200 • C for 1 h under dynamic vacuum (p < 0.1 Pa). Phosphorus trichloride (Sigma-Aldrich, 99%) was used without further purification.
• C for 12 h under vacuum. To remove even traces of water for the synchrotron experiments, the ILs were dried at 70 • C for 24 h, at 110 • C for 12 h and finally at 200 • C for 1 h under dynamic vacuum (p < 0.1 Pa). Phosphorus trichloride (Sigma-Aldrich, 99%) was used without further purification.
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