Desiccant efficiency in solvent and reagent drying. 5. Amines

Burfield, David R.; Smithers, Roger H.; Tan, Andrew

doi:10.1021/jo00316a030

Cited by 41 publications

(15 citation statements)

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“…The thermal behavior was determined by simultaneous DTA/TG analyses exemplarily for the coordination polymers ∞ 1 [Nd 2 Cl 6 (dpe) 2 (thz) 4 ]·dpe ( 2 ), ∞ 1 [GdCl 3 (dpe)(py) 2 ]·(dpe/py) ( 3 ), ∞ 1 [DyCl 3 (dpe)(thz) 2 ]·(dpe/thz) ( 8 ) and ∞ 1 [HoCl 3 (dpe)(thz) 2 ]·thz ( 11 ). Knowledge of melting and boiling points of dpe (mp = 150–153 °C and bp = 334 °C), thiazole (mp = −31 °C, bp = 117–118 °C) and pyridine (bp = 114 °C) allows assignment of the differential thermal analysis (DTA)/thermogravimetric (TG) signals of the compounds. All investigated compounds show rather similar thermal behavior with three defined mass losses around 150, 340, and 500 °C, indicating related transformation and decomposition processes.…”

Section: Resultsmentioning

confidence: 99%

Near-Infrared Luminescence and Inner Filter Effects of Lanthanide Coordination Polymers with 1,2-Di(4-pyridyl)ethylene

et al. 2016

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A series of 12 lanthanide coordination polymers was synthesized from anhydrous LnCl 3 and 1,2-di(4-pyridyl)ethylene (dpe) under solvothermal conditions in either thiazole (thz) or pyridine (py). The reactions yielded ∞ 1 [Ln 2 Cl 6 (dpe) 2 (thz) 4 ]•dpe with Ln = Ce (1), Nd (2), ∞ 1 [LnCl 3 (dpe)(py) 2 ]•(dpe/py) with Ln = Gd (3), Er (4), and ∞ 1 [LnCl 3 (dpe) (thz) 2 ](dpe/thz) with Ln = Sm (5), Gd (6), Tb (7), Dy (8), Er (9), Yb (10), as well as ∞ 1 [HoCl 3 (dpe)(thz) 2 ]•thz (11) and ∞ 2 [La 2 Cl 6 (dpe) 3 (py) 2 ]•dpe ( 12). One-dimensional coordination polymers (CPs) and a two-dimensional network of five different constitutions are formed by connection of LnCl 3 units via dpe molecules. As free ligand, dpe shows an excimer effect that is reduced in the coordination polymers. In addition, dipyridylethylene proves to be a suitable sensitizer for the photoluminescence of lanthanides in the near-infrared region (NIR) only. Thereby, dpe differs from the related ligand 1,2-di(4-pyridyl)ethane. For the compounds presented, four different luminescence effects were detected: luminescence based on fluorescence of the linker dpe is observed in the visible region, whereas ligand-sensitized 4f−4f NIR emission is dominating for trivalent Nd, Er, and Yb. The Er-containing CPs show an inner-filter effect of Er 3+ , which is based on reabsorption of emission of dpe triggering the erbium NIR emission.

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Section: Resultsmentioning

confidence: 99%

Near-Infrared Luminescence and Inner Filter Effects of Lanthanide Coordination Polymers with 1,2-Di(4-pyridyl)ethylene

et al. 2016

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“…Pyridine was dried with a short column of activated alumina and stored over 3 Å molecular sieves under inert atmosphere for 2 days prior to use. 21 2-and 3-Hydroxypyridines were dried by dissolving 300 mg samples in 2 mL of anhydrous methanol and passing the yellow mixture through a Pasteur pipet ¾ full of activated alumina (~1.25 g). After rinsing the column with additional solvent (2 mL), the colorless solution was concentrated with a rotary evaporator and then a mechanical pump (0.1 torr), and the remaining white solid was stored in a glovebox.…”

Section: Generalmentioning

confidence: 99%

Structural considerations for charge‐enhanced Brønsted acid catalysts

Payne

Kass

2020

J of Physical Organic Chem

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All three N-methylated and N-protonated hydroxypyridinium BAr F 4 salt isomers were synthesized and their hydrogen bond donating abilities were investigated. DFT and G4 theory computations along with IR spectroscopic measurements were found to be effective methods for predicting the catalytic activities of these O-H and N-H Brønsted acids. A UV-vis titration approach for rapidly quantifying hydrogen bond donating ability revealed that carbonhydrogen bonds also can participate in electrostatic interactions, but the presence of multiple equilibrium complexes results in a limitation of this method. In the methylated series of hydroxypyridines, the ortho and para isomers displayed modest rate enhancements relative to the meta derivative. Protonation introduces a new acidic site and the ortho hydroxypyridinium ion This article is protected by copyright. All rights reserved. This is the author manuscript accepted for publication and has undergone full peer review but has not been through the copyediting, typesetting, pagination and proofreading process, which may lead to differences between this version and the Version of Record. Please cite this article as

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“…Technical problems emerge when applying the distillation approach, as both liquid and vapour hydrazine are quite explosive. The drying-agent approach was performed using KOH [23], CaH 2 [17], BaO [24], and molecular sieves [25]. The effectiveness of a drying agent was assessed by qualitative reaction with trimethoxysilane or by recording a 1 H-NMR spectrum.…”

Section: Resultsmentioning

confidence: 99%

A new method for the synthesis of 3-hydrazinopropyl trimethoxysilane

Põhako¹,

Saal²,

Bredihhin³

et al. 2011

Proc. Estonian Acad. Sci.

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A new method for the synthesis of 3-hydrazinopropyl trimethoxysilane is proposed. The method is relatively simple and is based on hydrosilylation like the synthesis of analogous aminosilanes. For drying allylhydrazine hydrate a new efficient silyl hydride base method is proposed. The product, a new hydrazino-ormosil (organically modified silicate), can be applied in chemical modification of SiO 2 surfaces, thus offering an alternative to aminosilane modification, which is widely applied in several surface coating technologies.

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Desiccant efficiency in solvent and reagent drying. 5. Amines

Cited by 41 publications

References 1 publication

Near-Infrared Luminescence and Inner Filter Effects of Lanthanide Coordination Polymers with 1,2-Di(4-pyridyl)ethylene

Near-Infrared Luminescence and Inner Filter Effects of Lanthanide Coordination Polymers with 1,2-Di(4-pyridyl)ethylene

Structural considerations for charge‐enhanced Brønsted acid catalysts

A new method for the synthesis of 3-hydrazinopropyl trimethoxysilane

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