Manipulation of air and/or moisture-sensitive compounds was done under a high-purity N2 atmosphere using standard Schlenk techniques. Toluene was routinely purified and distilled over Na before use. 1,2-dimethoxyethane (DME)–NiBr2 complex was synthesized by the reaction of DME with anhydrous NiBr2. Methylaluminoxane (MAO, 1.46 m solution in toluene) and modified Methylaluminoxane (MMAO, 1.93 m in n-heptane) were purchased from AkzoNobel. Trimethylaluminium (TMA, 1.00 m in toluene) was purchased from Aldrich. Me2AlCl (1.00 m in toluene) and other reagents were purchased from Acros Chemicals or local suppliers. Elemental analysis was completed by using a Flash EA 1112 microanalyzer (Thermo Fisher Scientific, Waltham, USA). FTIR spectra were determined by a System 2000 FTIR spectrometer (PerkinElmer, Waltham, USA). Gas chromatography (GC) analysis was performed with a CP-3800 gas chromatograph (Varian, Palo Alto, USA) equipped with a flame ionization detector and a 30 m column (0.2 mm internal diameter, 0.25 μm film thickness).
Methylaluminoxane
Manufactured by AkzoNobel
Sourced in China
Methylaluminoxane is a chemical compound used as a catalyst component in the production of polyolefins. It is a clear, colorless liquid with a characteristic odor. Methylaluminoxane is employed as a co-catalyst in the synthesis of various types of polymers.
Automatically generated - may contain errors
Lab products found in correlation
Modified methylaluminoxane, by AkzoNobel (3 mentions)
Cp 3800 gas chromatograph, by Agilent Technologies (2 mentions)
System 2000 ftir spectrometer, by PerkinElmer (1 mentions)
Flash ea 1112 microanalyzer, by Thermo Fisher Scientific (1 mentions)
600 mhz spectrometer, by Bruker (1 mentions)
400 mhz dmx instrument, by Bruker (1 mentions)
3 protocols using methylaluminoxane
1
Synthesis and Characterization of Air-Sensitive Compounds
2
Synthesis and Characterization of Air-Sensitive Organometallic Compounds
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All handling
of air- and humidity-sensitive compounds was conducted by using the
Schlenk technique or in an argon-filled MBRAUN glovebox. Prior to
use, organic solvents, such as toluene, n-hexane,
ether, and tetrahydrofuran, were dried over the fine sodium wires
and then refluxed with sodium/potassium benzophenone under nitrogen.
All polymerization grade ethylene, high-purity nitrogen (99.999%),
and high-purity argon (99.999%) were purchased from Jiangsu Hongren
Special Gas Co., Ltd. (China), and no further purification was carried
out. CH2Cl2 and CDCl3 were degassed
and dried over CaH2. Both methylaluminoxane (MAO, 10% solution
in toluene) and modified methylaluminoxane (MMAO, 7.1% aluminum solution
in toluene) were purchased from Akzo-Nobel company. Anhydrous CrCl3 and Cr(CO)6 were purchased from J & K Chemical
Technology Co. CrCl3(THF)3 was prepared by referring
to the procedures in the literature.31 (link)1H NMR, 13C{1H} NMR, 19F NMR, and 31P{1H} NMR spectra were recorded
on a Bruker 600 MHz spectrometer (Figures S1–S20 ). Melting points of compounds were measured in a sealed glass tube
of a Büchi-540 instrument. Elemental analysis was tested on
a Thermo Quest Italia SPA EA 1110 instrument.
of air- and humidity-sensitive compounds was conducted by using the
Schlenk technique or in an argon-filled MBRAUN glovebox. Prior to
use, organic solvents, such as toluene, n-hexane,
ether, and tetrahydrofuran, were dried over the fine sodium wires
and then refluxed with sodium/potassium benzophenone under nitrogen.
All polymerization grade ethylene, high-purity nitrogen (99.999%),
and high-purity argon (99.999%) were purchased from Jiangsu Hongren
Special Gas Co., Ltd. (China), and no further purification was carried
out. CH2Cl2 and CDCl3 were degassed
and dried over CaH2. Both methylaluminoxane (MAO, 10% solution
in toluene) and modified methylaluminoxane (MMAO, 7.1% aluminum solution
in toluene) were purchased from Akzo-Nobel company. Anhydrous CrCl3 and Cr(CO)6 were purchased from J & K Chemical
Technology Co. CrCl3(THF)3 was prepared by referring
to the procedures in the literature.31 (link)1H NMR, 13C{1H} NMR, 19F NMR, and 31P{1H} NMR spectra were recorded
on a Bruker 600 MHz spectrometer (
of a Büchi-540 instrument. Elemental analysis was tested on
a Thermo Quest Italia SPA EA 1110 instrument.
3
Synthesis and Characterization of Nickel Complexes
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All manipulations involving air and moisture-sensitive compounds were carried out under an atmosphere of purified nitrogen using standard Schlenk. Toluene was dried over sodium metal and distilled under nitrogen. Methylaluminoxane (MAO, 1.46 M solution in toluene) and modified Methylaluminoxane (MMAO, 1.93 M in heptane) were purchased from Akzo Nobel Corp. (Nanjing, China). Diethylaluminium chloride (Et2AlCl, 1.17 M in hexane) and ethylaluminium sesquichloride (EASC, 0.87 M in hexane), triethylaluminium (Et3Al, 2.00 M in heptane) and other reagents were purchased from Acros Chemicals (Beijing, China). (DME)NiBr2 was synthesized by the reaction of 1,2-dimethoxyethane with anhydrous nickel(II) bromide. FT-IR spectra were recorded on a Perkine-Elmer System 2000 FT-IR spectrometer (Shanghai, China). Elemental analysis was carried out using a Flash EA 1112 microanalyzer (Beijing, China). 1H- and 13C-NMR spectra were recorded on a Bruker DMX 400 MHz instrument (Beijing, China) at ambient temperature using tetramethylsilane (TMS) as an internal standard. GC analyses were performed with a Varian CP-3800 gas chromatograph (Beijing, China) equipped with a flame ionization detector and a 30 m (0.2 mm i.d., 0.25 mm film thickness) CP-Sil 5 CB column.
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