542-56-3Relevant articles and documents
Preparation method of 4-(BOC-amino)-1-butanol
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Paragraph 0051; 0053; 0058; 0060; 0065; 0067, (2021/01/28)
The invention discloses a preparation method of 4-(BOC-amino)-1-butanol. The method comprises the following steps: reacting a proper amount of 2, 3-dihydrofuran with an acidic solution to obtain 2, 3-dihydro-5-methyl furan; mixing the obtained 2, 3-dihydro-5-methyl furan with hydrochloride, and then adding the mixture into an alkaline solution for reaction to obtain isobutyl nitrite; reacting isobutyl nitrite under the action of a reducing agent to generate 4-amino-1-butyl alcohol; and reacting 4-amino-1-butyl alcohol with di-tert-butyl dicarbonate in tetrahydrofuran to generate 4-(BOC-amino)-1-butyl alcohol; according to the preparation method of the 4-(BOC-amino)-1-butanol, the total yield of the product is as high as 70%, the reaction temperature is low, and the safety coefficient is high), the reducing agent is cheaper than that in the prior art, the experimental operation method is simple, the steps are short, and the method is suitable for large-scale production.
Spectrokinetic study of the reaction system of 2NO2?N 2O4 with butanols between 320-358 K in the gas phase
Wojcik-Pastuszka,Jodkowski
experimental part, p. 131 - 143 (2009/09/25)
Spectrokinetic studies of the gas-phase equilibrium between nitrogen tetroxide and butanols in the reaction system 2NO2?N 2O4 (1,2), N2O4+ROH? RONO+HNO3 (3,4) have been undertaken in the temperature range 298-358 K. The products - RONO (n-butyl-ONO, sec-butyl-ONO, iso-butyl-ONO and tert-butyl-ONO) - were identified by their UV spectra and the values of the maxima UV absorption cross sections were determined in the range 320-420 nm at 298 K. The temperature dependences of both the forward and reverse rate constants, k3 and k4, were obtained. The extrapolated values of the forward rate constants are 10-18 k3 av/cm3 molec-1 s-1 3.9±1.0; 1.7±0.3; 4.2±0.8; 5.7±1.1 and the reverse rate constants are 10-20 k4av/cm3 molec -1 s-1 0.3±0.1; 2.3±0.6; 0.4±0.1; 2.3±0.6 at 298 K for the reaction of NO2/N2O 4 with n-butanol, sec-butanol, iso-butanol and tert-butanol, respectively. The activation energy for the forward E3 and for the reverse E4 reaction were derived.
Reaction of alcohol with NO2 on a Cleaned Glass Surface
Maeda, Yasuaki,Fujio, Yoshifumi,Munemori, Makoto
, p. 2127 - 2130 (2007/10/02)
Formation of alkyl nitrite from alcohol and NO2 was very fast on a Pyrex glass surface cleaned with chromic acid mixture.The reaction was practically zero order with respect to NO2.The rate constant was (1.7 +/- 0.08)*10E-18 cm3*molecule-1*s-1 for methyl nitrile formation and the apparent activation energy was -53.5 kJ*mol-1.
Disproportionation to Combination Ratios of Alkoxy Radicals with Nitric Oxide
Morabito, Paul,Heicklen, Julian
, p. 2914 - 2916 (2007/10/02)
The disproportionation to combination ratios were measured at 175 deg C for the reactions RO + 15NO -> RO15NO (2a) and RO + 15NO -> RCHO + H15NO (2b), with the following alkoxy radicals: C2H5O, n-C3H7O, n-C4H9O, and i-C4H9O.The alkoxy radical was generated by the termal decomposition of the corresponding alkyl nitrite in the presence of 15NO.The rate of the corresponding isotopically enriched alkyl nitrite was measured by mass spectrometry while the aldehyde rate was determined by gas chromatography.The results obtained for k2b/k2 were 0.22 +/= 0.02, 0.26 +/= 0.03, 0.29 +/= 005, and 033 +/= 0.03, respectively, for C2H5O, n-C3H7O, n-C4H9O, and i-C4H9O.With these values of k2b/k2 we were able to determine the primary quantum yield of the photolysis of the corresponding alkyl nitrites at 366 nm to be, respectively, 0.32 +/= 0.04, 0.44 +/= 0.06, 0.19 +/= 0.04, and 0.19 +/= 0.02.
A kinetic study of the influence of alcohols on the nitrosation of morpholine in acid media. Equilibrium constants for the formation of alkyl nitrites
Casado, Julio,Lorenzo, Francisco Manuel,Mosquera, Manuel,Prieto, Maria Flor Rodriguez
, p. 136 - 138 (2007/10/02)
The effect of the aliphatic alcohols methanol, ethanol, propanol, isopropanol, 2-butanol, isobutanol, and tert-butanol on the rate of nitrosation of morpholine at pH 3 and 25 deg C has been studied.The inhibition observed is attributed to the formation of alkyl nitrites, which are poor nitrosating agents in acid media.The equilibrium constants for the formation of alkyl nitrites from nitrous acid and alcohols have been calculated both spectrophotometrically and from kinetic data for the inhibitory effect, and there is agreement between the two sets of results.The molar absorptivities at 265 nm of the alkyl nitrites have also been determined.When the concentration of alkyl nitrite is very low, a slight catalytic effect considered to be an effect of the medium has been observed.
Hydrolysis, Nitrosyl Exchange, and Synthesis of Alkyl Nitrites
Doyle, Michael P.,Terpstra, Jan W.,Pickering, Ruth A.,LePoire, Diane M.
, p. 3379 - 3382 (2007/10/02)
Alkyl nitrites undergo relatively slow hydrolysis in phosphate-buffered aqueous media under neutral conditions with small but significant dependence of reactivity on structure.However, rapid nitrosyl exchange with alcohols is observed, and equilibrium constants for this transformation exhibit remarkable correlation with equilibrium constants for nitrosyl exchange of alcohols with nitrosyl chloride and with nitrous acid. tert-Butyl nitrite has the greatest driving force for nitrosyl transfer among the 12 alkyl nitrites examined, and this capability is used for the synthesis of alkyl nitrites derived from steroidal alcohols and of alkyl thionitrites.
Gas-phase Reaction of Hydroxyl Radicals with Alkyl Nitrite Vapors in H2O2+NO2+CO Mixtures
Audley, Gary J.,Baulch, Donald L.,Campbell, Ian M.,Waters, Des J.,Watling, Gillian
, p. 611 - 618 (2007/10/02)
The yields of CO2 from the chain reaction in H2O2+NO2+CO+alkyl nitrite mixtures, in wich OH is the chain carrier and alkyl nitrites induce a chain termination step, have been used to deduce rate constants (ks) for OH attack on alkyl nitrites (RONO) in the vapour phase at ambient temperatures.Values of ks/E9 dm3 mol-1 s-1 as a function of R were determined as follows: 0.71 +/-0.12 (CH3), 1.15+/-0.23 (C2H5), 1.56+/-0.32 (n-C3H7), 3.41+/-1.48 (n-C4H9), 3.89+/-0.58 (sec-C4H9), 3.47+/-0.52 (i-C4H9), 0.91+/-0.15 (t-C4H9), all based on ks=(1.63+/-0.16)E9 dm3 mol-1 s-1 for OH +n-butane.The small increase in ks from R=CH3 to t-4H9 is considered to support a recent postulate that both H-abstraction and NO-abstraction pathways are operative, at least for R=CH3.Under typical, sunlit urban atmosphere conditions it is deduced that OH attack on alkyl nitrites is a minor removal process compared to their photodissociative destruction.
