Showing papers on "Tetrahydrofuran published in 1974"
01 Jul 1974
TL;DR: In this article, a spectral and calorimetric investigation was carried out into hydrogen bonding between the surface hydroxyl groups of silica and molecules of n -hexane, cyclohexane and carbon tetrachloride, benzene, nitromethane, acetonitrile, acetone, diethyl ether, dioxane, tetrahydrofuran, pyridine, and triethylamine.
Abstract: A spectral and calorimetric investigation was carried out into hydrogen bonding between the surface hydroxyl groups of silica and molecules of n -hexane, cyclohexane, carbon tetrachloride, benzene, nitromethane, acetonitrile, acetone, diethyl ether, dioxane, tetrahydrofuran, pyridine, and triethylamine. The integral intensity of the absorption band due to the stretching vibration of free hydroxyl groups on the surface of aerosil and the integral intensities of the absorption bands of these hydroxyl groups perturbed by adsorbed molecules were determined. From the difference in the heats of adsorption on hydroxylated and strongly dehydroxylated surfaces of a pure macroporous silica the heats of formation of the hydrogen bond between adsorbed molecules and free surface hydroxyl groups were evaluated. They were compared with the change in the integral intensity of the stretching vibration band of the hydroxyl groups resulting from adsorption and with their frequency shifts. The relation between the spectral and energetic characteristics of the hydrogen bond resulting from adsorption is approximately the same as that which occurs when the hydrogen bond is formed in solution.
166 citations
TL;DR: In this article, Butyllithium is not suitable as metalating reagent for metal-substituted carbenes and C-metalated Diazoalkanes.
64 citations
TL;DR: The thermal stability of the Grignard reagent and the products of the thermal decomposition have been estimated in diethyl ether and tetrahydrofuran as mentioned in this paper.
55 citations
TL;DR: The thermal decomposition of compounds of the type Cp 2 TiR 2 (Cp = cyclopentadienyl, R = aryl or benzyl) in the solid state and in various solvents has been studied.
53 citations
TL;DR: In this article, the reaction of α-Metalated Diethyl Isocyanomethyl- and α-Isocyanobenzylphosphonates with carbonyl compounds was studied.
50 citations
TL;DR: Prenyllithium and cis-crotyllithium react with carbonyl compounds to give the branched alcoholates with moderate to high selectivity, unless access to the carbonyls group is strongly hindered as mentioned in this paper.
Abstract: Prenyllithium (3-methylbut-2-enyl-lithium) (1) and cis-crotyllithium (Z-but-2-enyl-lithium) (2) in tetrahydrofuran solution, prepared according to the method of Eisch & Jacobs, react with carbonyl compounds to give the branched alcoholates with moderate to high selectivity, unless access to the carbonyl group is strongly hindered (see the Table). Adamantanethione (12) reacts with 1 to give the unbranched thiolate.
49 citations
TL;DR: In this paper, the authors investigated the kinetics of anionic polymerization of methylmethacrylate in tetrahydrofuran at −75 and showed that the polymerization proceeds practically without side reactions under these conditions.
48 citations
TL;DR: The key step of the title synthesis involves the conversion of ethyl trimethylsilylacetate to the corresponding enolate, 1, by treatment with lithium dicyclohexylamide in tetrahydrofuran at −78 °C.
Abstract: The key step of the title synthesis involves the conversion of ethyl trimethylsilylacetate to the corresponding enolate, 1, by treatment with lithium dicyclohexylamide in tetrahydrofuran at −78 °C. The condensation of 1 with aldehydes and ketones proceeds smoothly to afford the desired two carbon homologated unsaturated esters in excellent yields. The new process is extended with success to readily-enolizable carbonyl compounds and also to chalcone, which gives no trace of the Michael adduct in the present reaction.
46 citations
TL;DR: In this article, various perfluoro-aliphatic Grignard reagents have been reacted with H 3 O +, CO 2, (CF 3 ) 2 CO and cyclohexanone to yield R f H, R f CO 2 H and 1-cyclo-C 6 H 10 (OH)R f compounds.
45 citations
43 citations
Patent•
25 Jan 1974
TL;DR: In this article, a method of producing butene-1 resides in dimerizing ethylene in the presence of a complex organometallic catalyst of the formula (RO)3 TiR'.
Abstract: The present invention relates to a method of producing butene-1. According to the invention, the method of producing butene-1 resides in dimerizing ethylene in the presence of a complex organometallic catalyst of the formula (RO)3 TiR' .AlR2 "OR + AlR2 "R', where R is an alkyl radical with from 2 to 4 carbon atoms, R' = R or H, R" is the same as R, or a catalyst having the formula Ti(OR)4 + AlR2 "R' and modifiers such as (C5 H5)2 TiCl2, oxygen, metaphenylenediamine or N-phenyl-β-naphthylamine, in the medium of solvents such as n-heptane, n-decane, toluene, diethyl ether, ethyl chloride, vinylbutyl ether, tetrahydrofuran, diphenyl ether, methylphenyl ether and mixtures thereof. The invention will find application in petrochemical processing.
Patent•
06 Jun 1974TL;DR: In this paper, the tetrahydrofuran polycarboxylic acids represented by the formula wherein R1, R2, R3, R4, R5 and R6 are hydrogen or carboxyly acid groups, at least one of R 1, R 2, R 3 and R 4 being a carboxyl acid group when R 5 is a carbo-cyclic acid group are useful as complexing agents and/or detergency builders.
Abstract: Salts of tetrahydrofuran polycarboxylic acids represented by the formula wherein R1, R2, R3, R4 and R5 are hydrogen or carboxylic acid groups, at least one of R1, R2, R3 and R4 being a carboxylic acid group when R5 is a carboxylic acid group are useful as complexing agents and/or detergency builders. The ester forms of such compounds, as well as the acids are useful as intermediates for production of the salts.
TL;DR: In this paper, it was shown that the optical spectra of tetrahydrofuran can be rationalized in terms of tight and loose ion pair-crown ether complexes.
Abstract: Bathochromic shifts observed in the optical spectra of alkali picrates in tetrahydrofuran on addition of crown ethers and bis-(crown ethers) can be rationalized in terms of tight and loose ion pair-crown ether complexes.
TL;DR: In this paper, the first 1-oxa-2-silacyclohexanes were synthesized from magnesium halide-catalyzed reactions of some dichlorosilanes and magnesium metal in tetrahydrofuran.
TL;DR: In this paper, the reaction of sodium [NN′-ethylenebis(salicylideneiminato)cobaltate(I)] with carbon dioxide in both tetrahydrofuran and pyridine gave the reversible adducts: Co(salen)CO2Na and (py)Co[salen] CO2Na, respectively, containing CO2 as the reduced species and in bent form.
Abstract: The reaction of sodium [NN′-ethylenebis(salicylideneiminato)cobaltate(I)] with carbon dioxide in both tetrahydrofuran and pyridine gave the reversible adducts: Co(salen)CO2Na and (py)Co(salen)CO2Na, respectively, containing CO2 as the reduced species and in bent form.
Patent•
22 Apr 1974TL;DR: A nonaqueous cell utilizing a highly active metal anode, such as lithium, a solid (CFx)n cathode and a liquid organic electrolyte based on 3-methyl-2-oxazolidone in combination with a low viscosity cosolvent such as tetrahydrofuran, and a metal salt selected from the group consisting of MBF4, MClO4 and MM''F6 wherein M is lithium, sodium or potassium and M'' is phosphorus, arsenic or antimony as mentioned in this paper.
Abstract: A nonaqueous cell utilizing a highly active metal anode, such as lithium, a solid (CFx)n cathode and a liquid organic electrolyte based on 3-methyl-2-oxazolidone in combination with a low viscosity cosolvent, such as tetrahydrofuran, and a metal salt selected from the group consisting of MBF4, MClO4 and MM''F6 wherein M is lithium, sodium or potassium and M'' is phosphorus, arsenic or antimony.
TL;DR: In this article, the reaction of TiCl3,3thf with potentially quadridentate Schiff's bases gives the complexes trichloro[NN′-ethylenebis(salicylideneimine)]tetrahydrofurantitanium(III), (I), dichloro [NN′]-ethylene bis(SalicylIDeneiminato)]titanium[IV, (II), (III), and trichchloro[N′-(o-hydroxybenzylamino-o-phenylene)
Abstract: Reaction of TiCl3,3thf (thf = tetrahydrofuran) with potentially quadridentate Schiff's bases gives the complexes trichloro[NN′-ethylenebis(salicylideneimine)]tetrahydrofurantitanium(III), (I), dichloro[NN′-ethylenebis(salicylideneiminato)]titanium(IV), (II), dichloro[NN′-o-phenylenebis(salicylideneiminato)]titanium(IV), (III), and trichloro[NN′-(o-hydroxybenzylamino-o-phenylene)salicylideneiminato]tetrahydrofurantitanium(IV), (IV). Hydrogenation of one of the CN bonds of the Schiff's base occurs in formation of complex (IV).
TL;DR: π-Cyclopentadienyl-1,2-bis(diphenylphosphino)-ethane iron bromide and magnesium in tetrahydrofuran (THF) afford the novel crystalline inorganic magnesium reagent (π-C5H5)(diphos)FeMgBr,3THF, containing a covalent iron-magnesium bond as discussed by the authors.
Abstract: π-Cyclopentadienyl-1,2-bis(diphenylphosphino)-ethane iron bromide and magnesium in tetrahydrofuran (THF) afford the novel crystalline inorganic magnesium reagent (π-C5H5)(diphos)FeMgBr,3THF, containing a covalent iron-magnesium bond (Fe–Mg 2·59 A).
TL;DR: In this article, synthetic zeolites were found to be effective catalysts for the ring transformation of tetrahydrofuran (THF) into pyrrolidine.
TL;DR: In this paper, photo-induced nitrosylation of Mn 2 (CO) 10 in n-pentane solution results in the formation of Mn(NO) 3 CO via Mn(CO) 4 NO, while complete decarbonylation is observed in tetrahydrofuran.
TL;DR: In this paper, a poly(dimethylsilyl)benzenes have been prepared by in situ reactions of polybromobenzenes with magnesium and dimethylchlorosilane in tetrahydrofuran.
Abstract: Poly(dimethylsilyl)benzenes have been prepared by ‘in situ’ reactions of polybromobenzenes with magnesium and dimethylchlorosilane in tetrahydrofuran. The hydrolysis of these compounds yields benzo[c][1,2,5]oxadisiloles.
TL;DR: In this paper, 1-Diazo-1-phenylathan (2) reacts with dicarbonyl(cyclopentadienyl)(tetrahydrofuran)mangenese (1a) and dic-binearl(methylcyclopentaddienyl) to ganese to yield the acetophenone imine complexes 5a and b, respectively.
Abstract: 1-Diazo-1-phenylethan (2) reagiert mit Dicarbonyl(cyclopentadienyl)(tetrahydrofuran)mangan (1a) bzw. Dicarbonyl(methylcyclopentadienyl)(tetrahydrofuran)mangan (1b) zu den Acetophenonimin-Komplexen 5a-bzw. b, IR- und 1H-NMR-spektroskopische Befunde machen die Koordination des Imin-Liganden uber das Stickstoff-Atom an das Metall wahrscheinlich. 5a wurde anhand seines Fragmentierungsschemas auch massenspektroskopisch gesichert.
Ketimine Complexes from 1-Diazo-1-phenylethane
1-Diazo-1-phenylathan (2) reacts with dicarbonyl(cyclopentadienyl)(tetrahydrofuran)mangenese (1a) and dicarbonyl(methylcyclopentadienyl)(tetrahydrofuran) manganese (1b) to ganese (1b) to yield the acetophenone imine complexes 5a and b, respectively. I.r. and 1H n.m.r. spectroscopic results indicate, that the imine ligand is co-ordinated with the nitrogen atom to the metal. 5a also was established by its mass spectroscopic fragmentation scheme.
TL;DR: In this paper, the 1H n.m.r. spectra of dihydrido-complexes were described, particularly the solvent dependent spectroscopic properties of these complexes.
Abstract: The complexes mer-[Re(S2CNR2)(N2)(PMe2Ph)3](I; R = Me or Et) have been prepared from trans-[ReCl(N2)(PMe2Ph)4] and Na[S2CNR2]. With an excess of HX (X = Cl or Br) in tetrahydrofuran (thf) solution they give the dihydrido-complexes [ReH2(S2CNR2)X(PMe2Ph)3]X, (II), which on treatment with NEt3 give [ReH(S2CNR2)X(PMe2Ph)3], (III). Complexes (III) give [ReH(S2CNR2)2(PMe2Ph)2], (IV), on reaction with Na[S2CNR2]. The spectroscopic properties of these complexes are described, particularly the 1H n.m.r. spectra which are solvent dependent. The complexes mer-[ Re(L)(N2)(PMe2Ph)3](L = S2COEt or S2PPh2) have also been prepared.
TL;DR: In this paper, a solution of an α,β-unsaturated ketone and methyl iodide in tetrahydrofuran was shown to lead to the α-monoalkylated compound.