A reaction mixture of Zn-MOF 2 (17.3 mg, 0.0157 mmol), 4-NBA (0.1511 g, 1.0 mmol), and trimethylsilyl cyanide (TMSCN, 0.125 mL, 1.0 mmol) in dry toluene (10 mL) in a screw-capped vial was heated under constant stirring (200 rpm) at 50 °C for 24 h. The reaction mixture was then filtered through a glass frit, and the solid was washed with chloroform and acetone. The solvent was removed from the filtrate by rotary evaporation, and the residue was dried under high vacuum and then completely dissolved in a mixture of CDCl3 and acetone-d6 (~45 mL). An internal standard, 1,1,2,2-tetrachloroethane (1.0 mmol, Sigma-Aldrich), was added to the deuterated solvent. The product was analyzed by 1H NMR spectroscopy. A distinct chemical shift at 5.6 ppm was observed for the cyanohydrin trimethylsilyl ether product. The signals were assigned by comparing the chemical shifts observed for the product with literature values.
1 1 2 2 tetrachloroethane
Manufactured by Merck Group
1,1,2,2-tetrachloroethane is a colorless, dense liquid that is commonly used as a laboratory reagent and solvent. It has a high boiling point and is a good solvent for various organic compounds. The chemical formula for 1,1,2,2-tetrachloroethane is C2H2Cl4.
Automatically generated - may contain errors
Lab products found in correlation
K2co3, by Merck Group (1 mentions)
Caco3, by Merck Group (1 mentions)
1 methyl 2 pyrrolidinone nmp, by Merck Group (1 mentions)
Benzoyl peroxide, by Merck Group (1 mentions)
Methyl iodide, by Merck Group (1 mentions)
N bromosuccinimide, by Merck Group (1 mentions)
N n dimethylacetamide dmac, by Merck Group (1 mentions)
Sncl4, by Merck Group (1 mentions)
Bis 4 fluorophenyl sulfone, by Merck Group (1 mentions)
4 4 dihydroxybiphenyl, by Merck Group (1 mentions)
Zncl2, by Merck Group (1 mentions)
Cs2co3, by Merck Group (1 mentions)
Cdcl3, by Merck Group (1 mentions)
Deuterated chloroform cdcl3, by Merck Group (1 mentions)
Azobisisobutyronitrile, by Merck Group (1 mentions)
Hydrochloric acid (hcl), by Samchun (1 mentions)
Fluoroethylene carbonate, by Merck Group (1 mentions)
Cdcl3, by Cambridge Isotopes (1 mentions)
1 methyl 2 pyrrolidinone, by Merck Group (1 mentions)
1 m lipf6, by Merck Group (1 mentions)
5 protocols using 1 1 2 2 tetrachloroethane
1
Synthesis of Cyanohydrin Trimethylsilyl Ether
2
Synthesis and Characterization of Anion Exchange Membranes
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ZnCl2, SnCl4, CMME, benzoyl peroxide (BPO), azobisisobutyronitrile (AIBN), N-bromosuccinimide (NBS), 1,1,2,2-tetrachloroethane (TCE), CDCl3, polysulfone (PSU) random copolymer (average Mn ∼ 22 000), bis(4-fluorophenyl) sulfone (DFDPS), 4,4′-(hexafluoroisopropylidene)diphenol (6F-BPA), 4,4′-dihydroxybiphenyl (BP), methyl iodide, Cs2CO3, K2CO3, CaCO3, deuterated chloroform (CDCl3) and N,N-dimethylsulfoxide (DMSO-d6), 1-methyl-2-pyrrolidinone (NMP), and N,N-dimethylacetamide (DMAc) were purchased from Sigma-Aldrich. Sodium chloride (NaCl), methanol and hydrochloric acid were supplied by Samchun Chemicals and used as received. Tetra(trimethylaminemethylene)-4,4′-dihydroxydiphenylether (TADHDPE) was synthesized following our previous report.27 (link) The FAA-3-30 membrane was purchased from FUMATECH as a reference AEM, and prior to its use, the counter ion was converted to chloride anion using aqueous 1 M NaCl solution.
3
Synthesis of Conjugated Heterocycles via Zn-MOF Catalysis
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A reaction mixture of Zn-MOF 2 (17.3 mg, 0.0157 mmol), an aldehyde of choice (1.0 mmol), and ethyl cyanoacetate (0.107 mL, 1.0 mmol) in dry toluene (10 mL) in a screw-capped vial was heated under constant stirring (200 rpm) at 50 °C for 48 h. The reaction mixture was filtered through a glass frit, and the solid residue was washed with chloroform and acetone. The solvent was removed from the filtrate by rotary evaporation, and the residue was dried under high vacuum and then completely dissolved in a mixture of CDCl3 and acetone-d6 (~10 mL). An internal standard, 1,1,2,2-tetrachloroethane (1.0 mmol, Sigma-Aldrich), was added to the deuterated solvent. The product was analyzed by 1H NMR spectroscopy by comparing the vinylic proton resonance signal approximately at 8.20 ppm and the signal of the internal standard at 5.95 ppm.
4
Synthesis and Characterization of Lithium-Ion Battery Materials
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Li2CO3 (99.99%, trace metals basis), 1 M LiPF6 in ethylene carbonate:dimethyl carbonate (EC:DMC 1:1 v/v, LP30, battery grade), fluoroethylene carbonate (FEC, 99%), 1-methyl-2-pyrrolidinone (NMP, anhydrous, 99.5%), 1,1,2,2-tetrachloroethane (TCE, ≥98.0%), and KBr (≥99.0%) were purchased from Sigma-Aldrich. Prior to use, FEC was dried over molecular sieves in an Ar-filled glovebox (O2 <0.1 ppm, H2O <0.5 ppm) for 48 h. KBr was dried in vacuo at 100°C for 3 days before bringing into the glovebox for use. All other chemicals were used as received. RuO2 (99.95%, trace metals basis) was purchased from Alfa Aesar and dried at 300°C for 4 h to remove moisture prior to syntheses. Carbon Super P and polyvinyldene fluoride (PVDF) were purchased from MTI Corporation and used as received. TEKPol was purchased from CortecNet; CDCl3 was purchased from Cambridge Isotope Laboratories, both were used as received.
5
Synthesis and Characterization of Triaryl Trisamines
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The triaryl trisamines 28 designated as TATA in what follows (see Fig. 1) were synthesised as described in ref. 28-30. As shown in these references these molecules pile up to form helical structures that further aggregate to produce fibrillar or elongated morphologies.
Due to steric hindrance the phenyl groups are tilted which entails the existence of a helical chirality when TATA moleculare are stacked.
1,1,2,2,-tetrachloroethane (TCE), 1,2-dichloroethane (DCE), 1,1,2,2-tetrabromoethane (TBE) and toluene were purchased from SigmaAldrich (purity grade 99.5%), and were used without further purification.
The TATA/solvent systems are obtained from mixtures prepared at the desired concentration, and then heated up to the appropriate temperature so as to make clear, homogeneous solutions. These solutions are then quenched at low temperature (0 1C down to À20 1C depending on the solvent) for producing the organized systems.
TATA concentrations are in the range from 0.5 Â 10 À2 g cm À3 to 0.12 g cm À3 for all the solvents. These concentrations are further expressed in weigh/weight in the temperature concentration phase diagrams, and therefore the w/w concentration range depends upon the solvent's density.
Due to steric hindrance the phenyl groups are tilted which entails the existence of a helical chirality when TATA moleculare are stacked.
1,1,2,2,-tetrachloroethane (TCE), 1,2-dichloroethane (DCE), 1,1,2,2-tetrabromoethane (TBE) and toluene were purchased from SigmaAldrich (purity grade 99.5%), and were used without further purification.
The TATA/solvent systems are obtained from mixtures prepared at the desired concentration, and then heated up to the appropriate temperature so as to make clear, homogeneous solutions. These solutions are then quenched at low temperature (0 1C down to À20 1C depending on the solvent) for producing the organized systems.
TATA concentrations are in the range from 0.5 Â 10 À2 g cm À3 to 0.12 g cm À3 for all the solvents. These concentrations are further expressed in weigh/weight in the temperature concentration phase diagrams, and therefore the w/w concentration range depends upon the solvent's density.
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