- H/D scrambling in a chromium-catalyzed dehydrocoupling reaction of a borane-dimethylamine adduct
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H/D scrambling took place in a chromium-catalyzed dehydrocoupling reaction of a deuterium-labeled borane-dimethylamine adduct. In the hydrogen elimination of BH3·NDMe2 (1a-dN), H2, HD and D2 were generated in 65:30:5 ratio, and 62% of deuterium atoms were incorporated into the major product, the dimethylaminoborane dimer. Proton and deuteron nuclei were thus concentrated into the evolved dihydrogen and aminoborane dimer, respectively. The mechanism of H/D scrambling is understood based on the reaction pathway of the dehydrocoupling of 1a, which was previously proposed based on DFT calculations. The H/D distribution in the products is explained by the energy difference according to the deuterated position in an intermediate of the dehydrocoupling reaction.
- Kawano, Yasuro,Shimoi, Mamoru
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Read Online
- Pressure-induced structural changes in Methylamine borane and dimethylamine borane
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Methylamine borane and dimethylamine borane have been studied under compression to 3 GPa using Raman spectroscopy and synchrotron powder X-ray diffraction. Both undergo reversible pressure-induced structural changes in this pressure range. The structural changes in the case of methylamine borane may be indicative of a second-order phase transition, taking place between ca. 0.8–1.2 GPa, which does not result in a change of space-group symmetry. In the case of dimethylamine borane, however, a reversible, reconstructive phase transition (monoclinic → orthorhombic) occurs below 0.7 GPa. This new high-pressure phase was successfully indexed, with a possible space group assignment of Pccn or Pbcn.
- Szilágyi, Petra á.,Hunter, Steven,Morrison, Carole A.,Tang, Chiu C.,Pulham, Colin R.
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Read Online
- The reaction of mono- and dimethylamines with phosphorus trifluoride borane
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The reaction between F3PBH3 and CH3NH2 gives [CH3NH]F2PBH3, [CH3NH]2FPBH3, or [CH3NH]3PBH3 depending upon the experimental conditions used. In no case was CH3NH2BH3 ever detected as a product of the methylamine reaction. On the other hand the reaction between F3PBH3 and (CH3)2NH gave good yields of (CH3)2NHBH3 under conditions comparable to those used for methylamine, and gave [(CH3)2N]F2PBH3 or [(CH3)2N]2FPBH3 under more severe conditions. Displacement reactions provide a basis for listing the above bases in order of increasing base strength using BH3 as a reference acid. The order is: F3P 3NH)F2P, [(CH3)2N]F2P 3)3, NH(CH3)2 3NH)2FP, [(CH3)2N]2FP. The results are discussed.
- Kodama,Parry
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Read Online
- Visible light-mediated synthesis of amides from carboxylic acids and amine-boranes
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Here, a photocatalytic deoxygenative amidation protocol using readily available amine-boranes and carboxylic acids is described. This approach features mild conditions, moderate-to-good yields, easy scale-up, and up to 62 examples of functionalized amides with diverse substituents. The synthetic robustness of this method was also demonstrated by its application in the late-stage functionalization of several pharmaceutical molecules.
- Chen, Xuenian,Kang, Jia-Xin,Ma, Yan-Na,Miao, Yu-Qi
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supporting information
p. 3595 - 3599
(2021/06/06)
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- Preparation method of dimethylamine borane
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The invention discloses a preparation method of dimethylamine borane, which comprises the following step of in a solvent, in the presence of monopotassium phosphate or phosphoric acid, reacting dimethylamine or hydrochloride thereof with BH4 ion-containing hydroboron to obtain the dimethylamine borane. The solvent is water or a mixed solvent of water and an organic solvent. The preparation method of dimethylamine borane disclosed by the invention is mild in condition, high in yield, high in purity and clean in reaction.
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Paragraph 0032-0089
(2021/06/12)
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- Amine-boranes as Dual-Purpose Reagents for Direct Amidation of Carboxylic Acids
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Amine-boranes serve as dual-purpose reagents for direct amidation, activating aliphatic and aromatic carboxylic acids and, subsequently, delivering amines to provide the corresponding amides in up to 99% yields. Delivery of gaseous or low-boiling amines as their borane complexes provides a major advantage over existing methodologies. Utilizing amine-boranes containing borane incompatible functionalities allows for the preparation of functionalized amides. An intermolecular mechanism proceeding through a triacyloxyborane-amine complex is proposed.
- Choudhary, Shivani,Hamann, Henry J.,Ramachandran, P. Veeraraghavan
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supporting information
(2020/11/13)
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- Method for the production of amine borane complex (by machine translation)
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The invention belongs to the technical field of material preparation, in particular relates to a method for the production of amine borane complex. This invention adopts the borane amine of the direct reaction of an inert gas stream, by regulating the ratio of the two, the need for further post-processing, to make the final product amine complex and offer. In the reaction process such impurity is introduced into the salt-free, does not use an organic solvent; the use of borohydride such as the reagent to produce the borane, for now the current system, can avoid direct operation of toxic gas borane. The method of the invention is simple in operation, the product has high purity, low cost, and can be continuous large-scale production. At the same time, the method and other way to produce the amine borane complex equipment compatible, production equipment by simple method can be used to adjust the production. (by machine translation)
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Paragraph 0035; 0036
(2017/12/05)
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- Catalytic Dehydrocoupling of Amine-Boranes using Cationic Zirconium(IV)-Phosphine Frustrated Lewis Pairs
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A series of novel, intramolecular Zr(IV)/P frustrated Lewis pairs (FLPs) based on cationic zirconocene fragments with a variety of ancillary cyclopentadienyl and 2-phosphinoaryloxide (-O(C6H4)PR2, R = tBu and 3,5-CF3-(C6H3)) ligands are reported and their activity as catalysts for the dehydrocoupling of dimethylamine-borane (Me2NH·BH3) assessed. The FLP system [(C9H7)2ZrO(C6H4)PtBu2][B(C6F5)4] is shown to give unprecedented turnover frequencies (TOF) for a catalyst based on a group 4 metal (TOF ≥ 600 h-1), while also proving to be the most efficient FLP catalyst reported to date. The mechanism of this reaction has been probed using analogous intermolecular Zr(IV)/P FLPs, permitting deconvolution of the reactions taking place at both the Lewis acidic and basic sites. Elucidation of this mechanism revealed an interesting cooperative two-cycle process where one cycle is FLP mediated and the other, a redistribution of a linear diborazane intermediate, relies solely on the presence of a Zr(IV) Lewis acid.
- Metters, Owen J.,Flynn, Stephanie R.,Dowds, Christiana K.,Sparkes, Hazel A.,Manners, Ian,Wass, Duncan F.
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p. 6601 - 6611
(2016/10/14)
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- B-Methylated Amine-Boranes: Substituent Redistribution, Catalytic Dehydrogenation, and Facile Metal-Free Hydrogen Transfer Reactions
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Although the dehydrogenation chemistry of amine-boranes substituted at nitrogen has attracted considerable attention, much less is known about the reactivity of their B-substituted analogues. When the B-methylated amine-borane adducts, RR'NH·BH2Me (1a: R = R' = H; 1b: R = Me, R' = H; 1c: R = R' = Me; 1d: R = R' = iPr), were heated to 70 °C in solution (THF or toluene), redistribution reactions were observed involving the apparent scrambling of the methyl and hydrogen substituents on boron to afford a mixture of the species RR'NH·BH3-xMex (x = 0-3). These reactions were postulated to arise via amine-borane dissociation followed by the reversible formation of diborane intermediates and adduct reformation. Dehydrocoupling of 1a-1d with Rh(I), Ir(III), and Ni(0) precatalysts in THF at 20 °C resulted in an array of products, including aminoborane RR'N=BHMe, cyclic diborazane [RR'N-BHMe]2, and borazine [RN-BMe]3 based on analysis by in situ 11B NMR spectroscopy, with peak assignments further supported by density functional theory (DFT) calculations. Significantly, very rapid, metal-free hydrogen transfer between 1a and the monomeric aminoborane, iPr2N=BH2, to yield iPr2NH·BH3 (together with dehydrogenation products derived from 1a) was complete within only 10 min at 20 °C in THF, substantially faster than for the N-substituted analogue MeNH2·BH3. DFT calculations revealed that the hydrogen transfer proceeded via a concerted mechanism through a cyclic six-membered transition state analogous to that previously reported for the reaction of the N-dimethyl species Me2NH·BH3 and iPr2N=BH2. However, as a result of the presence of an electron donating methyl substituent on boron rather than on nitrogen, the process was more thermodynamically favorable and the activation energy barrier was reduced.
- Stubbs, Naomi E.,Sch?fer, Andr,Robertson, Alasdair P.M.,Leitao, Erin M.,Jurca, Titel,Sparkes, Hazel A.,Woodall, Christopher H.,Haddow, Mairi F.,Manners, Ian
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supporting information
p. 10878 - 10889
(2015/11/27)
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- Rehydrogenation of aminoboranes to amine-boranes using H2O: Reaction scope and mechanism
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Water has been successfully employed as a reagent with which to rehydrogenate aminoboranes (e.g., iPr2N=BH2, 2,2,6,6-Me4C5H6N=BH2, and also transient Me2N=BH2 derived from 1/2[Me2N-BH2]2) to amine-boranes (e.g., iPr2NH·BH3, 2,2,6,6-Me4C5H6NH·BH3, Me2NH·BH3) in approximately 30 yield. The conversion to amine-boranes from the corresponding aminoboranes using this method represents an example of a metal-free, single-step route for the hydrogenation of the B=N bond. Deuterium labeling studies indicated that the protic hydrogen (N-H) on the rehydrogenated amine-borane was derived from H2O, whereas the third hydridic hydrogen (B-H) on the amine-borane was generated from the formation of a postulated hydride-bridged intermediate H2B(μ-H)(μ-NR2)B(OH)H (R2 = Me2, iPr2, 2,2,6,6-Me4C5H6), which requires a second equivalent of the starting aminoborane, thus explaining the low yield. Formation of insoluble borates (BxOyHz) provides a driving force for the reaction. Significantly, the yield can be increased by adding a sacrificial source of BH3 (e.g., to ca. 53% for BH3·THF) or by adding a separate source of H- (e.g., to ca. 95% for LiBH4) to complement the H+ (from H2O) in a more atom-efficient reaction.
- Leitao, Erin M.,Manners, Ian
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supporting information
p. 2199 - 2205
(2015/05/13)
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- Synthesis and the thermal and catalytic dehydrogenation reactions of amine-thioboranes
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A series of trimethylamine-thioborane adducts, Me3N· BH2SR (R = tBu [2a], nBu [2b], iPr [2c], Ph [2d], C6F 5 [2e]) have been prepared and characterized. Attempts to access secondary and primary amine adducts of thioboranes via amine-exchange reactions involving these species proved unsuccessful, with the thiolate moiety shown to be vulnerable to displacement by free amine. However, treatment of the arylthioboranes, [BH2-SPh]3 (9) and C6F 5SBH2·SMe2 (10) with Me2NH and iPr2NH successfully yielded the adducts Me2NH· BH2SR (R = Ph [11a], C6F5 [12a]) and iPr 2NH·BH2SR (R = Ph [11b], C6F5 [12b]) in high yield. These adducts were also shown to be accessible via thermally induced hydrothiolation of the aminoboranes Me2N=BH 2, derived from the cyclic dimer [Me2N-BH 2]2 (13), and iPr2N=BH2 (14), respectively. Attempts to prepare the aliphatic thiolate substituted adducts R2NH·BH2SR′ (R = Me, iPr; R′ = tBu, nBu, iPr) via this method, however, proved unsuccessful, with the temperatures required to facilitate hydrothiolation also inducing thermal dehydrogenation of the amine-thioborane products to form aminothioboranes, R2N= BH(SR′). Thermal and catalytic dehydrogenation of the targeted amine-thioboranes, 11a/11b and 12a/12b were also investigated. Adducts 11b and 12b were cleanly dehydrogenated to yield iPr2N=BH(SPh) (22) and iPr2N=BH(SC6F5) (23), respectively, at 100 °C (18 h, toluene), with dehydrogenation also possible at 20 °C (42 h, toluene) with a 2 mol % loading of [Rh(μ-Cl)cod]2 in the case of the former species. Similar studies with adduct 11a evidenced a competitive elimination of H2 and HSPh upon thermolysis, and other complex reactivity under catalytic conditions, whereas the fluorinated analogue 12a was found to be resistant to dehydrogenation.
- Robertson, Alasdair P. M.,Haddow, Mairi F.,Manners, Ian
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scheme or table
p. 8254 - 8264
(2012/09/22)
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- Mechanism of metal-free hydrogen transfer between amine-boranes and aminoboranes
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The kinetics of the metal-free hydrogen transfer from amine-borane Me 2NH?BH3 to aminoborane iPr2N=BH 2, yielding iPr2NH?BH3 and cyclodiborazane [Me2N-BH2]2 via transient Me 2N=BH2, have been investigated in detail, with further information derived from isotopic labeling and DFT computations. The approach of the system toward equilibrium was monitored in both directions by 11B{1H} NMR spectroscopy in a range of solvents and at variable temperatures in THF. Simulation of the resulting temporal-concentration data according to a simple two-stage hydrogen transfer/dimerization process yielded the rate constants and thermodynamic parameters attending both equilibria. At ambient temperature, the bimolecular hydrogen transfer is slightly endergonic in the forward direction (ΔG1° (295) = 10 ± 7 kJ?mol-1; ΔG 1(295) = 91 ± 5 kJ?mol-1), with the overall equilibrium being driven forward by the subsequent exergonic dimerization of the aminoborane Me2N=BH2 (ΔG 2°(295) = -28 ± 14 kJ?mol-1). Systematic deuterium labeling of the NH and BH moieties in Me 2NH?BH3 and iPr2N=BH2 allowed the kinetic isotope effects (KIEs) attending the hydrogen transfer to be determined. A small inverse KIE at boron (kH/kD = 0.9 ± 0.2) and a large normal KIE at nitrogen (kH/kD = 6.7 ± 0.9) are consistent with either a pre-equilibrium involving a B-to-B hydrogen transfer or a concerted but asynchronous hydrogen transfer via a cyclic six-membered transition state in which the B-to-B hydrogen transfer is highly advanced. DFT calculations are fully consistent with a concerted but asynchronous process.
- Leitao, Erin M.,Stubbs, Naomi E.,Robertson, Alasdair P. M.,Helten, Holger,Cox, Robert J.,Lloyd-Jones, Guy C.,Manners, Ian
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p. 16805 - 16816
(2013/01/15)
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- Catalytic redistribution and polymerization of diborazanes: Unexpected observation of metal-free hydrogen transfer between aminoboranes and amine-boranes
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Ir-catalyzed (20 °C) or thermal (70 °C) dehydrocoupling of the linear diborazane MeNH2-BH2-NHMe-BH3 led to the formation of poly- or oligoaminoboranes [MeNH-BH2]x (x = 3 to >1000) via an initial redistribution process that forms MeNH 2?BH3 and also transient MeNH=BH2, which exists in the predominantly metal-bound and free forms, respectively. Studies of analogous chemistry led to the discovery of metal-free hydrogenation of the B=N bond in the "model" aminoborane iPr2N=BH2 to give iPr2NH?BH3 upon treatment with the diborazane Me3N-BH2-NHMe-BH3 or amine-boranes RR′NH?BH3 (R, R′ = H or Me).
- Robertson, Alasdair P. M.,Leitao, Erin M.,Manners, Ian
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supporting information; experimental part
p. 19322 - 19325
(2012/01/13)
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- An inexpensive procedure for reductive aminations using dimethylamineborane on millimolar and molar scale
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We have developed an inexpensive and easy procedure for reductive aminations using dimethylamineborane instead of cyanoborohydride. Dimethylamineborane is easily prepared from readily available inexpensive starting materials and can be used without isolat
- Ortmann, Regina,Schlitzer, Martin
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experimental part
p. 1757 - 1759
(2009/12/25)
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- Structures and aggregation of the methylamine-borane molecules, Me nH3-nN BH3 (n = 1-3), studied by X-ray diffraction, gas-phase electron diffraction, and quantum chemical calculations
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The structures of the molecules methylamine-borane, MeH2 ? BH3, and dimethylamine-borane, Me2HN? BH3, have been investigated by gas-phase electron diffraction (GED) and quantum chemical calculations. The crystal structures have also been determined for methylamine-, dimethylamine-, and trimethylamine-borane, MenH 3-nN ? BH3 (n = 1-3); these are noteworthy for what they reveal about the intermolecular interactions and, particularly, the N-H...H-B dihydrogen bonding in the cases where n = 1 or 2. Hence, structures are now known for all the members of the ammonia- and amine-borane series MenH3-nN?BH3 (n = 0-3) in both the gas and solid phases. The structur al variations and energetics of formation of the gaseous adducts are discussed in relation to the basicity of the Me nH3-nN fragment. The relative importance of secondary interactions in the solid adducts with n = 0-3 has been assessed by the semi-classical density sums (SCDS-PIXEL) approach.
- Aldridge, Simon,Downs, Anthony J.,Tang, Christina Y.,Parsons, Simon,Clarke, Michael C.,et al.
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experimental part
p. 2231 - 2243
(2009/07/30)
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- Dehydrocoupling reactions of borane-secondary and -primary amine adducts catalyzed by group-6 carbonyl complexes: Formation of aminoboranes and borazines
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Photoirradiation of a solution of BH3·NHR2 (1a: R = Me, 1b: R = 1/2C4H8, 1c: R = 1/2C 5H10, 1f: R = Et) containing a catalytic amount of a group-6 metal carbonyl complex, [M(CO)6] (M = Cr, Mo, W), led to dehydrogenative B-N covalent bond formation to produce aminoborane dimers, [BH2NR2]2 (2a-c, f), in high yield. During these reactions a borane σ complex, [M(CO)5(η1- BH3·NHR2)] (3), was detected by NMR spectroscopy. Similar catalytic dehydrogenation of bulkier amineboranes, BH 3·NHiPr2 (1d) and BH3· NHCy2 (1e, Cy = cyclo-C6H11), afforded monomeric products BH2=NR2 (4d, e). The reaction mechanism of the dehydrocoupling was investigated by DFT calculations. On the basis of the computational study, we propose that the catalytic dehydrogenation reactions proceed via an intramolecular pathway and that the active catalyst is [Cr(CO)4]. The reaction follows a stepwise mechanism involving NH and BH activation. Dehydrocoupling of borane-primary amine adducts BH 3·NH2R (1g: R = Me, 1h: R = Et, 1i: R = tBu) gave borazine derivatives [BHNR]3 (5g-i).
- Kawano, Yasuro,Uruichi, Mikio,Shimoi, Mamoru,Taki, Seitaro,Kawaguchi, Takayuki,Kakizawa, Taeko,Ogino, Hiroshi
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p. 14946 - 14957
(2010/01/16)
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- Process for producing organic amine borane compounds
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The invention provides an improved process for preparing organic amine borane complex characterized in that it takes advantage of the slow reaction of potassium borohydride with water and the increased solubility in an ether/water mixed solvent containing minor amount of sodium hydroxide, adding slowly an organic amine to control the reaction rate and effectively control the generation of hydrogen gas in a manner to increase the yield and ensure the process safety.
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- Metal Tetrahydroborates and Tetrahydroborato Metalates, 15. An 11B and 113Cd NMR Study of MBH4-CdCl2 Systems in Dimethylformamide and the X-Ray Structure of CdCl2 * 2 DMF
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CdCl2 dissociates in dimethylformamide into the species Cd(DMF)62+, CdCl(DMF)5+ and CdCl3- as determined by 113Cd NMR spectroscopy. 11B and 113Cd NMR spectra of MBH4/CdCl2 solutions in this solvent show the presence of complexes - with rapid exchange of BH4- and Cl- at ambient temperature.There is no evidence that Cd(BH4)2 is formed in a metathetical reaction.The crystal structure of CdCl2 * 2 DMF has been determined.It is a coordination polymer containing hexacoordinated Cd atoms with the DMF molecules in cis-position.Coordination of DMF occurs via the carbonyl oxygen atoms.
- Linti, Gerald,Noeth, Heinrich,Thomann, Martina
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p. 1463 - 1471
(2007/10/02)
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- 13C nuclear magnetic resonance studies of aromatic amine-borane adducts
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13C NMR measurements are reported for 22 aromatic amine-borane, 7 aliphatic amine-borane, and 3 aliphatic amine-trimethylborane adducts.Additivity of the substituent effects on the δ 13C values of the aromatic carbon atoms is observed.The δ 13C values are compared with those of the arylamines of arylammonium salts and of corresponding alkyl-substituted benzenes.The δ 13C values for the borane adducts, ammonium salts and hydrocarbons exhibit the same trends.However, in the borane adducts similar to the ammonium salts, part of the shielding of the ortho-carbon atoms is attributed to electric field effects which are much less pronounced in the hydrocarbon analogues.The comparison of δ 13C values of aliphatic amine-borane adducts with those of corresponding hydrocarbons indicates the importance of steric effects.
- Paz-Sandoval, M. A.,Camacho, C.,Contreras, R.,Wrackmeyer, B.
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p. 1331 - 1336
(2007/10/02)
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- NMR studies of the reactions of Me2AsH with Me2AsNMe2 and Me2AsNMe2·BH3: Synthetic routes to Me2AsAsMe2
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Me2AsH reacts irreversibly with Me2AsNMe2 and Me2AsNMe2·BH3 to give good yields of Me2AsAsMe2. The nitrogen-containing product is Me2NH or Me2NH·BH3, respectively. These reactions have been followed by using multinuclear (1H, 11B, and 13C) NMR spectroscopy to elucidate the respective reaction mechanisms. Although the Me2AsH/Me2AsNMe2 reaction proceeds faster initially, the overall rate of reaction is slower than that for the Me2AsH/Me2AsNMe2·BH3 reaction. This is a consequence of the presence of inhibiting exchange reactions in the Me2AsH/Me2AsNMe2 system that are absent when Me2AsNMe2 and Me2NH are bound to BH3 in the Me2AsH/Me2AsNMe2·BH3 reaction. A detailed NMR study of the exchange reactions involving the >AsNNH, >AsAsAsH, and >AsNAsAs2AsAsMe2.
- Gupta, Virendra K.,Krannich, Larry K.,Watkins, Charles L.
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p. 2553 - 2556
(2008/10/08)
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- A mechanistic model for the reactions of ammonia and the methylamines with phosphine-borane
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When H3PBH3 is dissolved in liquid ammonia at -45° and allowed to stand, the final product is the ionic solid, [NH4][H2P(BH3)2]. At temperatures above -45° increasing amounts of the covalent ammonia-borane, H3NBH3, are formed along with the ionic product, [NH4][H2P(BH3)2]. Methylamine and dimethylamine behave quite differently. At temperatures of -45° and below only the covalent amine-borane, [CH3H2NBH3] or [(CH3)2HNBH3], is obtained as a product. At temperatures above -45° increasing amounts of the ionic product, [CH3NH3][H2P(BH3)2] or [(CH3)2N-H2][H2P(BH 3)2], are found in the amineborane. It is significant that temperature effects are completely reversed in these two systems. Finally (CH3)3N gives only the covalent base addition compound, (CH3)3NBH3, under all conditions studied. A mechanistic model dealing with the anion H2PBH3- is advanced to interpret the above observations. Copyright 1976 by the American Chemical Society.
- Dietz Jr., Edward A.,Morse, Karen W.,Parry, Robert W.
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- Dialkylaminohydridophenoxyboranes. Convenient preparation and studies of intramolecular boron-nitrogen π bonding
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A convenient preparation of dialkylaminohydridophenoxyborane compounds (HBOC6H5NR'2) has been developed according to the following three-step sequence: (1) 4BF3 (etherate) + 3NaBH4 = 3NaBF4 + 2B2H6(g); (2) 1/2B2H6(g) + HNR'2 = H3BNHR'2; (3) H3BHNR'2 + HOC6H5 + heat = 2H2 + HBOC6H5NR'2; HNR'2 = HN(CH3)2, HN(C2H5)2, HN(i-C3H7)2, HN(n-C4H9)2, HN(CH2C6H5)2, HNC4H8, and HNC5H10. The final products are isolated in yields ranging from 70 to 90% by vacuum distillation at moderate temperatures. Molecular association and variable-temperature proton magnetic resonance studies of these compounds in benzene solution are consistent with a planar, monomeric configuration with considerable π interaction between boron and nitrogen and hindered rotation about this bond. The Lewis acid behavior of diisopropylaminohydridophenoxyborane toward ammonia and trimethylamine was determined using a tensimetric titration procedure. No evidence of interaction was observed with trimethylamine while a stable 1:1 adduct was formed in the case of the reaction involving ammonia: HBOC6H5N(i-C3H7)2 + NH3 = HBOC6H5N(i-C3H7)2-NH 3. The room-temperature proton magnetic resonance spectrum of the ammonia adduct of diisopropylaminohydridophenoxyborane has demonstrated relatively unrestricted rotation about the secondary amino nitrogen-boron bond.
- Kovar, Roger A.,Waldvogle, Gene G.
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p. 2239 - 2243
(2008/10/08)
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- Chemistry of boranes. XV. Synthesis of diborane from boric oxide
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A direct synthesis of diborane from boric oxide has been achieved by hydrogenation of the oxide in the presence of aluminum and aluminum trichloride. Very pure diborane is obtained from this reaction in 40-50% conversions at temperatures above 150° and hydrogen pressures of 750 atm. This hydrogenation is believed to proceed through an aluminum chlorohydride intermediate. Amine boranes, aminoboranes, and borazines were obtained directly from boric oxide when the hydrogenation was effected in the presence of secondary or tertiary alkylamines.
- Ford,Kalb,Mcclelland,Muetterties
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p. 1032 - 1035
(2008/10/08)
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