Synthesis of heterocyclic bromacetylene alcohols and their acryl -, methacryl ethers

The article presents a method for obtaining heterocyclic bromoacetylenic alcohols by the action of sodium hypobromide on cyclic and heterocyclic acetylene alcohols, as well as their acrylic and methacrylic esters using lithium aluminum complexes. The composition and structure of the obtained products were confirmed by the data of elemental analysis, IR and PMR spectra. As a result of the study, it was found that in the presence of lithium aluminum hydride, the product yield in all cases is higher than 80 %.

Green synthesis of graphite from CO2 without graphitization process of amorphous carbon

Environmentally benign synthesis of graphite at low temperatures is a great challenge in the absence of transition metal catalysts. Herein, we report a green and efficient approach of synthesizing graphite from carbon dioxide at ultralow temperatures in the absence of transition metal catalysts. Carbon dioxide is converted into graphite submicroflakes in the seconds timescale via reacting with lithium aluminum hydride as the mixture of carbon dioxide and lithium aluminum hydride is heated to as low as 126 °C. Gas pressure-dependent kinetic barriers for synthesizing graphite is demonstrated to be the major reason for our synthesis of graphite without the graphitization process of amorphous carbon. When serving as lithium storage materials, graphite submicroflakes exhibit excellent rate capability and cycling performance with a reversible capacity of ~320 mAh g–1 after 1500 cycles at 1.0 A g–1. This study provides an avenue to synthesize graphite from greenhouse gases at low temperatures.

Lithium aluminum hydride reduction of 1-phenylbutane-1,3-dione, and acetylation of the products: NMR and GC-MS analysis

Reduction of ?-diketones with lithium aluminum hydride (LiAlH4, LAH) can lead to different products, depending on the tautomeric equilibrium: the reduction of diketo forms gives the corresponding diols and the reduction of ketoenol forms yields elimination products, saturated and unsaturated ketones and alcohols. Here, we report on the results of LAH reduction of 1-phenylbutane-1,3-dione. The products of reduction were further acetylated and separated by dry flash chromatography. The obtained products, phenylbut(en)ols, phenylbut(en)ones and phenylbut(en)yl acetates, were characterized by spectral (1H and 13C NMR, MS) and retention index (RI) data. It can be concluded that LAH preferentially reduces the carbonyl group more distant from the phenyl group of 1-phenylbutane-1,3-dione. The structure-retention index relationships between isomers were discussed. Proton splitting patterns were resolved by proton NMR simulations.

Nucleophilic transformations of azido-containing carbonyl compounds via protection of azido group

Nucleophilic transformations of azido-containing carbonyl compounds are disclosed. The phosphazide formation from azides and di(tert-butyl)(4-(dimethylamino)phenyl)phosphine (Amphos) enabled transformations of carbonyl groups with nucleophiles such as lithium aluminum hydride and organometallic...

A New Zeolitic Lithium Aluminum Imidazolate Framework

An aliovalent mixed-metal framework DUT-174 [LiAl(2-methylimidazolate)4]n, isostructural to ZIF-8, was synthesized from lithium aluminum hydride (LiAlH4) and 2-methylimidazole (2-mImH) through dehydrogenation. Lithium and aluminum cations acting as alternating framework nodes...

Formation of an Isomeric Mixture of Dienynes Instead of a Diallene

Attempts to convert 1,1,2,2,7,7,8,8-octaethoxyocta-3,5-diyne to a symmetric allene by reduction with lithium aluminum hydride failed. Instead reduction accompanied by isomerization occurred and afforded 1,1,2,7,8,8-hexaethoxyocta-2,6-dien-4-yne as a mixture of three isomers in 63% total isolated yield.

Poly(2-ethyl-2-oxazoline-co-N-propylethylene imine)s by controlled partial reduction of poly(2-ethyl-2-oxazoline): Synthesis, characterization and cytotoxicity

The partial reduction of poly(2-ethyl-2-oxazoline) was investigated. A series of poly(2-ethyl-2-oxazoline-co-N-propylethylene imine)s were synthesized by direct reduction using lithium aluminum hydride or borane/dimethylsulfide (BH3/DMS), respectively. It is shown that the degree...