- Practical catalytic nitration directly with commercial nitric acid for the preparation of aliphatic nitroesters
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To pursue a sustainable and efficient approach for aliphatic nitroester preparation from alcohol, europium-triflate-catalyzed nitration, which directly uses commercial nitric acid, has been successfully developed. Gram scalability with operational ease showed its practicability.
- An, Jichao,He, Pan,Li, Wenhao,Liu, Peipei,Si, Mengyuan,Yang, Bo,Yang, Guanyu
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p. 6612 - 6616
(2020/09/21)
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- CONTINUOUS SYNTHESIS OF ISOOCTYL NITRATE IN A FLOW REACTOR
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A process for synthesizing isooctyl nitrate in a continuous flow reactor comprises flowing a H2SO4-HNO3 mixture within a flow reactor, flowing isooctyl alcohol into said flow reactor so as to mix the isooctyl alcohol with the H2SO4-HNO3 mixture and produce a reaction mixture stream flowing in said reactor, maintaining the reaction mixture stream flowing in said flow reactor at a reaction temperature within in the range -10° to 35°C inclusive, and wherein the residence time of the reaction mixture stream in the flow reactor is greater than or equal to 5 seconds and less than or equal to 40 seconds, and wherein the H2SO4 of the H2SO4-HNO3 mixture is H2SO4 having a concentration of in the range of 85 to 95% inclusive, more desirably 88 to 92% inclusive, most desirably of 90%.
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Paragraph 0029
(2015/09/28)
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- Process for the preparation of nitric esters of monohydric alcohols
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The present invention relates to a process for the preparation of nitric esters of monohydric alcohols wherein a monohydric alcohol or a mixture of monohydric alcohols is converted with nitric acid to the corresponding nitric esters under adiabatic reaction conditions in the presence of sulfuric acid.
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Page/Page column 4
(2008/06/13)
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- Clean nitrations: Novel syntheses of nitramines and nitrate esters by nitrodesilylation reactions using dinitrogen pentoxide (N2O5)
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In this novel nitration method dinitrogen pentoxide (N2O5) in an inert solvent is used as the nitrating agent, thereby removing the need for strong acids as the reaction medium. The N2O5 cleaves heteroatom-silicon bonds, in silylamines and silyl ethers respectively, to yield the desired energetic groupings (nitramines or nitrate esters respectively) without liberation of acids which would occur with conventional substrates (amines or alcohols). These nitrodesilylation reactions proceed cleanly and in good yield, and the scope of the reaction is illustrated by 29 examples, some of which produce high energy compounds, notably plasticisers and an energetic polymer precursor. These reactions are therefore potentially clean nitrations for the manufacture of energetic compounds which will minimise the impact of this activity on the environment in the future.
- Millar, Ross W.,Philbin, Simon P.
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p. 4371 - 4386
(2007/10/03)
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- Separation of Diastereomeric and Enantiomeric Alkyl Nitrates - Systematic Approach to Chiral Discrimination on Cyclodextrin LIPODEX-D
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High-resolution gas chromatographic separation of all diastereomeric monomethyl-substituted cyclohexyl nitrates is shown on a nonpolar methylpolysiloxane stationary phase, and the first application of this procedure to the environmental diastereomeric analysis of alkyl nitrates is presented.Two characteristic signals in the achiral analysis of atmospheric samples could be assigned to the smallest alkyl nitrate containing two asymmetric carbon atoms, 3-methyl-2-pentyl nitrate.Retention indices in the temperature-programmed separation based on the n-alkanes were determined.The homologous series of 1-alkyl nitrates were found to be useful as ECD-visible n-alkanes.Enantiomeric separation of alkyl nitrates was achieved on heptakis(3-O-acetyl,-2,6-di-O-pentyl)-β-cyclodextrin (LIPODEX-D).The influence of the nitrooxy group and the alkyl chain length on the chiral discrimination on LIPODEX-D is discussed for 25 chiral alkyl nitrates.The absolute configurations of some alkyl nitrates were assigned by asymmetric synthesis of enantiomerically pure references.The complexity of the alkyl nitrate mixtures present in air samoles does not allow a direct chiral separation as the alkyl nitrates partly coelute on the LIPODEX-D column.Column coupling of LIPODEX-D with a polar achiral stationary phase like polyalkylenglocol (PAG) was successfully applied to solve this problem, and the chiral alkyl nitrates present in a typical air sample were separated.A systematic nomenclature for alkyl nitrates is introduced to handle the steadily growing number of branched and long-chain nitrates detected in environmental analysis. - Keywords: analytical methods; alkyl nitrates; chiral resolution; cyclodextrins; gas chromatography
- Schneider, Manfred,Ballschmiter, Karlheinz
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p. 539 - 544
(2007/10/03)
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