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.
Labmaster dp
Manufactured by MBraun
The Labmaster dp is a laboratory glove box system designed for the control and monitoring of inert atmospheres. It provides a controlled environment for handling and processing air-sensitive materials.
Automatically generated - may contain errors
Lab products found in correlation
Lithium bromide, by Merck Group (1 mentions)
Copper 1 iodide, by Merck Group (1 mentions)
Lct premier mass spectrometer, by Waters Corporation (1 mentions)
Magnesium ribbon, by Merck Group (1 mentions)
Phosphorus trichloride, by Merck Group (1 mentions)
Avance dpx 400 mhz spectrometer, by Bruker (1 mentions)
2 protocols using labmaster dp
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
Synthesis of Air-Sensitive Organometallic Compounds
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All reactions were carried out under argon with the rigorous exclusion of air and water (< 5 ppm oxygen or water) using standard Schlenk-vessel and vacuum line techniques or a glovebox (recirculating mBraun LabMaster DP). Glassware was dried overnight at 60 °C before use. Solvents were thoroughly dried by standard methods and distilled immediately before use. 1 H, 13 (link) 190°C. Reaction is rapid at T ~ 500-600°C with a heat gun. TBD was obtained from Aldrich and recrystallized in toluene before use.
[TBD][Na], [25] [TBD-SiMe2][Cl] [19] , [TBD-BBN]2 [18] and HBCy2 [26] were synthesized according to literature procedures.
[TBD][Na], [25] [TBD-SiMe2][Cl] [19] , [TBD-BBN]2 [18] and HBCy2 [26] were synthesized according to literature procedures.
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