DubaiAmateurRocketry
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Synthesizing Organic Azides - DMAZ
So DMAZ, 2-DiMethylAminoethylaZide
is pretty interesting because it's not very detonable, as in, its not any primary explosives. It is though, somewhat hypergolic, when it comes in
contact with N2O4, HNO3(high conc), or HOOH.
Anyways, the synthesis of this compound is almost not described anywhere.
Any clues ?
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Tsjerk
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How is your German?
They make it with the chloride and sodium azide in water.
| Quote: | 6. Dimethyl-[B-azido-athyll-amin: 14.4 g (0.1 Mol) Dimethyl-[~-chlor-athylJ-amin-hydrochlorid
und 13.0g (0.2 Mol) Natriumazid wurden in 55ccm Wasser gelbst, 8 Stdn. im siedenden
Wasserbad envarmt (Braunfarbung). Nach 15stdg. Aufbewahren bei Raumtemp. wurde zur
ZerstSrung nicht umgesetzten Chloramins mit 4g NaOH in 15ccm Wasser versetzt und
21/2 Stdn. spater 7 Stdn. im Kutscher-Steudel-Apparat ausgeathert. Nach Verdampfen des
Athers und nach Dest. bei 40--M)" Badtemp./l6 Torr blieben neben geringen Mengen harzigen
Rilckstandes 5.04g (45% d.Th.) farbloses Azidoamin vom Sdp.16 32-40".
Pikrat: Mit methanol. Pikrimiiure in tiefgelben Nadeln vom Schmp. 114- 115" (nicht
umkristallisiert). |
Attachment: schiemenz1959.pdf (352kB)
This file has been downloaded 265 times
Edit: I don't know what "stdg." means... can't find it with google, maybe a typo meaning "stdn."? stdn. means "hours".
[Edited on 4-6-2018 by Tsjerk]
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DubaiAmateurRocketry
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Thanks for that, my german is bad, ill translate it.
I mean thats straightforward, going from 2-Chloro-N,N-dimethylethylamine, but how would one synthesize that?
Also, how would one synthesize azido-pentane? or azido-dioxane?
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Tsjerk
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If you have thionyl chloride:
( ((2-(Trimethylammonio)ethyl)thio)methyl)-2-(hydroxymethyl)-
pyridine Bromide (6). To 50 mL of thionyl chloride cooled at 0 OC was
slowly added 2-(dimethylamino)ethanol (2 g, 22.5 mmol). After the
addition, stirring was continued at room temperature for 12 h. The
thionyl chloride was then evaporated under reduced pressure, and the
residue was washed twice with toluene to give 2.97 g (92% yield) of
dimethyl(2-chloroethyl)amine hydrochloride, mp 201-203 "C (lit.29 mp
201.5-203 "C), which was not further purified:
Source: DOI: 10.1021/ja00183a034
Or via 2-chloro-ethanol (http://www.sciencemadness.org/talk/viewthread.php?tid=12607) and dimethyl-amine (citation needed)
Azido-pentane is straight forward; http://www.prepchem.com/synthesis-of-1-azidopentane/ (Edit: although you might want to find a source with a bit more OTC solvent, ethoxy-ethanol
is a bit OTC).
[Edited on 4-6-2018 by Tsjerk]
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