All manipulations were performed under inert conditions using either standard Schlenk techniques or nitrogen-filled glovebox. House nitrogen was purified through a MBraun HP-500-MO-OX gas purifier. nHexane, toluene and THF were purified by refluxing over potassium using benzophenone as an indicator and distilled prior to use. The chemicals pentamethylcyclopentadiene (Cp*H), allylmagnesium chloride (2.0 M in THF), potassium bistrimethylsilylamide (KN(Si(CH3)3)2), anhydrous YCl3, and 2.2.2-cryptand (crypt-222) were purchased from Sigma-Aldrich. 2.2.2-cryptand (crypt-222) was recrystallized from nhexane prior to use. KCp*,30 (link) (HNEt3)(BPh4),31 (link) Cp*2Y(BPh4),19 (link) H2Bbim,32 (link) (Li(TMEDA))2Bbim33 (link) and KC8 34 (link) were synthesized according to literature procedures.
2.2.2 cryptand crypt 222
Manufactured by Merck Group
2.2.2-cryptand (crypt-222) is a macrocyclic polyether compound commonly used as a complexing agent in organic synthesis and analytical chemistry. It is capable of forming stable complexes with a variety of cations, including alkali and alkaline earth metals. The core function of 2.2.2-cryptand is to act as a host molecule, selectively encapsulating and solubilizing guest species.
Automatically generated - may contain errors
3 protocols using 2.2.2 cryptand crypt 222
1
Inert Synthesis of Cyclopentadienyl Organometallics
2
Synthesis of Cationic Organolanthanide Complexes
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All manipulations were performed under inert conditions using either standard Schlenk techniques or argon-filled glovebox. nHexane, toluene and THF were purified by refluxing over potassium using benzophenone as an indicator and distilled prior to use. The chemicals pentamethylcyclopentadiene (Cp*H), allylmagnesium chloride (2.0 M in THF), potassium bistrimethylsilylamide (KN(Si(CH3)3)2) anhydrous LnCl3 (Ln = Gd, Tb, Dy), Celite, and 2.2.2-cryptand (crypt-222) were purchased from Sigma Aldrich. Crypt-222 was recrystallized from nhexane prior to use. KCp*,30 (link) (HNEt3)(BPh4),31 (link) Cp*2Ln(BPh4),26 (link) H2Bbim,32 (link) KC8 (ref. 33 (link)) and K2Bbim29 (link) were synthesized according to literature procedures.
3
Inert Atmosphere Synthesis Protocols
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All manipulations were performed
in either an argon- or nitrogen-filled MBraun glovebox with an atmosphere
of <0.1 ppm of O2 and <0.1 ppm of H2O.
House nitrogen was purified through an MBraun HP-500-MO-OX gas purifier.
Tetrahydrofuran (THF) was predried by refluxing over potassium for
several days, distilled, and stirred over Na/K alloy for final purification.
Dimethoxyethane (DME) and toluene were dried over potassium, and nhexane was dried over calcium hydride. All
solvents were distilled under N2 from their drying agents,
and water/oxygen absence was confirmed via benzophenone solution as
an indicator within a glovebox prior to use. Deuterated solvents were
purchased from Cambridge Isotope Laboratories, dried over Na/K alloy
for several days, and filtered prior to use. Anhydrous ErCl3 was purchased from Sigma-Aldrich and used as received. 2.2.2-Cryptand
(crypt-222) was purchased from Sigma-Aldrich and crystallized from
hot nhexane prior to use. Tetrabutylammonium
hexafluorophosphate [nBu4N][PF6] was purchased from Sigma-Aldrich and crystallized several
times before use. Dibenzocyclooctatetraene (dbCOT)40 (link) and potassium graphite (KC8)41 (link) were prepared according to literature procedures. Elemental
analysis was performed at Michigan State University using a PerkinElmer
2400 Series II CHNS/O analyzer.
in either an argon- or nitrogen-filled MBraun glovebox with an atmosphere
of <0.1 ppm of O2 and <0.1 ppm of H2O.
House nitrogen was purified through an MBraun HP-500-MO-OX gas purifier.
Tetrahydrofuran (THF) was predried by refluxing over potassium for
several days, distilled, and stirred over Na/K alloy for final purification.
Dimethoxyethane (DME) and toluene were dried over potassium, and nhexane was dried over calcium hydride. All
solvents were distilled under N2 from their drying agents,
and water/oxygen absence was confirmed via benzophenone solution as
an indicator within a glovebox prior to use. Deuterated solvents were
purchased from Cambridge Isotope Laboratories, dried over Na/K alloy
for several days, and filtered prior to use. Anhydrous ErCl3 was purchased from Sigma-Aldrich and used as received. 2.2.2-Cryptand
(crypt-222) was purchased from Sigma-Aldrich and crystallized from
hot nhexane prior to use. Tetrabutylammonium
hexafluorophosphate [nBu4N][PF6] was purchased from Sigma-Aldrich and crystallized several
times before use. Dibenzocyclooctatetraene (dbCOT)40 (link) and potassium graphite (KC8)41 (link) were prepared according to literature procedures. Elemental
analysis was performed at Michigan State University using a PerkinElmer
2400 Series II CHNS/O analyzer.
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