CN102924288B - Method for preparing and synthesizing ammonium salt - Google Patents
Method for preparing and synthesizing ammonium salt Download PDFInfo
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- CN102924288B CN102924288B CN 201210494497 CN201210494497A CN102924288B CN 102924288 B CN102924288 B CN 102924288B CN 201210494497 CN201210494497 CN 201210494497 CN 201210494497 A CN201210494497 A CN 201210494497A CN 102924288 B CN102924288 B CN 102924288B
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- toluene
- triethylamine
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Abstract
The invention discloses a method for synthesizing triethylamine hydrochloride. The method comprises the following steps of: dissolving 5ml of dimethyl dichlorosilance in 20ml of water and 20ml of toluene, heating and refluxing in a magnetic heating stirrer for 5 hours, extracting the obtained products by using CH2Cl2, and rotating subnatant to obtain liquid in which the solvent is removed; and dissolving the obtained liquid in 20ml of toluene, adding 10ml of triethylamine, reacting for 2 hours, stopping stirring, carrying out rotary evaporation to obtain white solid, preparing saturated solution through trichloromethane for solid, standing for a day, and separating out colorless transparent needle crystal.
Description
One, technical field
The present invention relates to a kind of preparation and synthetic method of ammonium salt, is exactly a kind of preparation and synthetic method of triethylamine hydrochloride.
Two, background technology
The synthetic method of ammonium salt has many bibliographical informations.As far back as 1956, J.Chem.Soc. reported the synthetic method of some ammonium salts, and nineteen fifty-nine, J.Am.Chem.Soc. has also reported the synthetic method of ammonium salt class.（1. Surrey, Alexander R.; Lesher, George Y.; Mayer, J. Richard; Webb, Wm. G. Journal of the American Chemical Society (1959), 81 2894-7; 2
. Davis, M. Journal of the Chemical Society (1956), 337-43.）。
In the experiment of applicant by the synthetic prestox four silica cyclic ethers of dimethyldichlorosilane(DMCS), obtained a kind of compound triethylamine dihydrochloride.
Three, summary of the invention
The present invention aims to provide the compound triethylamine hydrochloride, and technical problem to be solved is that one-step synthesis obtains target product.
The alleged a kind of triethylamine hydrochloride of the present invention be by dimethyldichlorosilane(DMCS) and water, toluene and triethylamine preparation by the compound shown in following chemical formula:
（Ⅰ） 。
Chemical name: triethylamine hydrochloride, be called for short compound (I).
The synthetic method of compound (I) comprises synthesizes and separates, and described synthesizing is that the 5ml dimethyldichlorosilane(DMCS) is dissolved in 20ml water and 20ml toluene, reflux 5h on the magnetic force heating stirrer, products therefrom CH
2Cl
2The liquid of subnatant rotation desolventizing is got in extraction.Gained liquid is dissolved in 20ml toluene again, adds the 10ml triethylamine, reacted 2 hours, stirring stops, and rotary evaporation gets white solid, and solid was joined saturated solution standing one day with trichloromethane, separates out the water white transparency needle-like crystal.
This reaction mechanism can be speculated as dimethyl disilane and water effect, generates dimethyl dihydroxyl silane and forms hydrogen bond with hydrochloric acid, and after adding triethylamine, rapid and hydrochloric acid forms the triethylamine hydrochloride crystal.
One step of this synthetic method obtains target product, and technique is simple, and is easy to operate.
Four, description of drawings
Fig. 1 is the X-diffraction analysis figure of triethylamine hydrochloride.
Five, embodiment
1. the synthetic method of triethylamine hydrochloride:
Measure the 5ml dimethyldichlorosilane(DMCS) and be dissolved in 20ml water and 20ml toluene, reflux 5h on the magnetic force heating stirrer, products therefrom CH
2Cl
2The liquid of subnatant rotation desolventizing is got in extraction.Gained liquid is dissolved in 20ml toluene again, adds the 10ml triethylamine, reacted 2 hours, stirring stops, and rotary evaporation gets white solid, and solid was joined saturated solution standing one day with trichloromethane, separates out the water white transparency needle-like crystal.Ultimate analysis: theoretical value: C:52.35% H:11.72% N:10.18%C: measured value: C:51.97% H:11.44% N:9.82%, IR spectrum 2940,2680,1477,1040,806.
The crystal structure determination of compound:
The monocrystalline of choosing suitable size at microscopically at room temperature carries out the experiment of X-ray single crystal diffraction, at the 293k temperature, on Oxford X-ray single crystal diffractometer, use through the MoKa of graphite monochromator monochromatization ray (λ=0.71073 A) and collect diffraction data with the w-Theta scan mode.The data obtained is carried out the Lp factor and experience absorption correction, and crystalline structure is solved by direct method, and diffraction data reduction and structure elucidation work use respectively SAINT-5.0 and SHELXS-97 program to complete.Crystal data is as follows:
Empirical formula C6 H16 N Cl
Molecular weight 137.65
Temperature 293 (2) K
Wavelength 0.71073 A
Crystallographic system, spacer triclinic(crystalline)system, P31c
Unit cell parameters a=8.3363 (18) A alpha=90 deg.
b = 8.3363(18) A beta = 90 deg.
c = 7.057(2) A gamma = 120 deg.
Volume 424.73(18) A^3
Electric density 2,1.076 Mg/m^3
Absorption correction parameter 0.366 mm^-1
Number of electrons 152 in unit cell
Crystallographic dimension 0.256 x 0.176x 0.123mm
Scope 2.82 to 25.49 at Theta angle
The index capture range of HKL-10＜=h＜=9 ,-8＜=k＜10 ,-8＜=l＜=8
Collection/independent diffraction data 2478/517 [R (int)=0.0315]
Data integrity degree 99.6 % of theta=30.5
The method Multi Slice Mode of absorption correction
Transmitance 1.00000 and 0.76768 of minimax
The Matrix least square method of the method F^2 that refine is used
Number/the number of parameters 517/2/27 of data number/use restriction
The method 1.206 that refine is used
The consistence factor R 1=0.0547 of point diffraction, wR2=0.1467
The identical factor R 1=0.0561 of observable diffraction, wR2=0.1492
The absolute configuration parameter-0.2(3)
Maximum summit on difference Fourier figure and peak valley 0.430 and-0.285e.A^-3
The typical bond distance's data of crystal:
N(1)-C(1) 1.495(6)
N(1)-C(1)#1 1.495(6)
N(1)-C(1)#2 1.495(6)
N(1)-H(1) 0.9100
C(1)-C(2) 1.464(9)
C(1)-H(1A) 0.9700
C(1)-H(1B) 0.9700
C(2)-H(2A) 0.9600
C(2)-H(2B) 0.9600
C(2)-H(2C) 0.9600
The typical bond angle data of crystal:
C(1)-N(1)-C(1)#1 112.0(5)
C(1)-N(1)-C(1)#2 112.0(5)
C(1)#1-N(1)-C(1)#2 112.0(5)
C(1)-N(1)-H(1) 106.9
C(1)#1-N(1)-H(1) 106.9
C(1)#2-N(1)-H(1) 106.9
C(2)-C(1)-N(1) 114.7(7)
C(2)-C(1)-H(1A) 108.6
N(1)-C(1)-H(1A) 108.6
C(2)-C(1)-H(1B) 108.6
N(1)-C(1)-H(1B) 108.6
H(1A)-C(1)-H(1B) 107.6
C(1)-C(2)-H(2A) 109.5
C(1)-C(2)-H(2B) 109.5
H(2A)-C(2)-H(2B) 109.5
C(1)-C(2)-H(2C) 109.5
H(2A)-C(2)-H(2C) 109.5
H(2B)-C(2)-H(2C) 109.5。
Claims (1)
1. the synthetic method of a triethylamine hydrochloride, comprise and synthesize and separate, and it is characterized in that: described synthesizing is that the 5ml dimethyldichlorosilane(DMCS) is dissolved in 20ml water and 20ml toluene, reflux 5h on the magnetic force heating stirrer, products therefrom CH
2Cl
2The liquid of subnatant rotation desolventizing is got in extraction; Gained liquid is dissolved in 20ml toluene again, adds the 10ml triethylamine, reacted 2 hours, stirring stops, and rotary evaporation gets white solid, and solid was joined saturated solution standing one day with trichloromethane, separates out the water white transparency needle-like crystal.
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Non-Patent Citations (6)
| Title |
|---|
| 2-氯乙胺盐酸盐的合成研究;鲁俊 等;《襄樊学院学报》;20060331;第27卷(第2期);36-37 * |
| 全氟辛酸钠与三甲胺及三乙胺盐酸盐混合体系的表面活性;朱瑶 等;《日用化学工业》;19980630(第3期);1-3 * |
| 朱瑶 等.全氟辛酸钠与三甲胺及三乙胺盐酸盐混合体系的表面活性.《日用化学工业》.1998,(第3期),1-3. |
| 盐酸三乙胺_三氯化铝离子液体催化酰基化合成乙酰水杨酰胺;陈维光;《精细石油化工 》;20091130;第26卷(第6期);19-20页 * |
| 陈维光.盐酸三乙胺_三氯化铝离子液体催化酰基化合成乙酰水杨酰胺.《精细石油化工 》.2009,第26卷(第6期),19-20页. |
| 鲁俊 等.2-氯乙胺盐酸盐的合成研究.《襄樊学院学报》.2006,第27卷(第2期),36-37. |
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