Trans ,4methylaminorex the real ice the king of of stims

Lordoftheshard

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Trans 4-Methylaminorex via Potassium Cyanate

Chemicals:
28.2 g (0.15 moles) (+/-) norephedrine-HCl. NOTE: (+/-) norephedrine-HCl and (+/-) norspeudoephedrine all fall under the rubric of PPA. You want norephedrine, not norspeudoephedrine.
12.0 g potassium cyanate (KOCN)
172 ml 2M hydrochloric acid (HCl)
20% sodium carbonate (Na2CO3)
Dichloromethane (DCM)
Distilled water (dH2O)

Equipment:
500 ml flat bottom flask
Magnetic hotplate with stir bar
Thermometer

Put 28.2 g PPA-HCl in about 150 ml dH2O in your 500 ml Erlenmeyer. It should all dissolve easily. Next add 12.0 g KOCN and magnetically stir. About 75% of the KOCN should dissolve readily. Reflux the mixture directly on your hotplate. Hotplate should just be hot enough to boil your mixture. At about 35 deg C, all the KOCN should dissolve. Reflux for about 2.5 hours, then allow to cool to room temp. First you should notice a clear oil precipitating to the top. Further cooling will precipitate white flakes on the bottom. Place the flask in your freezer for about ½ hour or until temp drops to 5 deg C. Pour the solution into a pyrex dish and slowly evaporate over low heat. Do not evaporate completely. Next, place the solution back in your washed Erlenmeyer and add about 275 ml dH2O. It should dissolve slightly. Magnetically stir and begin heating the solution. Add 172 ml of 2M HCl and continue stirring and heating until just boiling. At about 50-60 deg C the white solution should turn clear again. Reflux again for about 2.5 hours magnetically stirring the whole time. Allow to cool to room temp. White powder will appear.

Wash the solution 3 times with a small amount of DCM. Isolate the water phase and basify it with your 20% Na2CO3 until no more white powder precipitates. Gravity filter the white powder and allow to dry at room temp with a fan or in an oven at low temp. Your yield should be about 15.5 g (+/-) trans 4-MAR freebase. [Forms Hcl salt readily.]

To salt the product and make it a HCL you can not do it in the normal fashion you must add equal molar amounts of HCl acid to the freebase and add 10 times that amount of xylene and azeotrope distill the product once the distillation is finish wash the reaction mix twice with anhydrous acetone and place it the freezer so easy this synth and makes the best product meth is the poor man version of 4mar

Respect to the inventor of this synth Billy from Florida Aka BetterLivingGuy
 
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K-Cyanide

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Great! 2 thumbs up!(y)(y).

It will remain a mystery why meth prevailed over 4-MAR. Anyway, how do you prepare your PPA ? I guess the times are long gone, when PPA was ectracted from OTC pills. Via benzaldehyd and nitroethane condensation(in an alkali/alcohol solution) followed by Zn/sulphuric acid reduction?

Your posting reminded me of a method producing L-phenylacetylcarbinol (L-PAC) by biotransformation of benzaldehyd with yeast via fermentation. L-PAC can then be converted to PPA by reductive amination. I always wanted to try this method one day. Its exerts a certain fascination on me. Maybe is this a starting signal to finally give it a try. ;)
 

azides

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KCN and cyanide bromide would probably bee why mate 😆
 

testint

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Cyanogen bromide is not even sold as far as I know 😔... You have to make it as you need it .oh and watch that team kids
 

azides

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Correct Cyanogen bromide isn't sold and sounds LIKE SOME NASTY SHIT.

Cyanide + bromine yeah ok I could see every meth cook Westside of Mississippi make it 😆
 

Lordoftheshard

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We were smurfing our dogs at the vets to get incontinence tablets for dogs the tablets have ppa in them
Then my friend used to work as a sales rep.fot veterinary products we got his boss on side and were getting the tablets during stock take
And I was getting norephedrine from India and Germany untill the DEA fucked everything and put the clamp on company's
Lpac is the way if you want to make your own norephedrine
 

Stretcher5335

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Fermentation of Benzaldehydes... Sounds like everyone wants to do it but never does. And there are a lot of you looking for answwers when there isnt anyone able to give real life answers. As with any fermentation it all comes down to the medium, the Yeast and the temp. ALL INGREDIENTS LISTED ARE WEIGHED AND DILUTED IN WATER FOR THE PREP OF 800cm
Medium A Medium B Medium C
PEPTONE 4.8g PEPTONE 4.8 YEAST EXTRACT 4.8g
SODIUM PYRUVATE 49.3g SURCOSE 80g SURCROSE 80g
CITRIC ACID 8.4g CITRIC ACID 8.4g AMMONIUM SULPHATE 7.32g
MAGNESIUM SULPHATE 0.4g PH NEEDS TO 4.5 FOR BOTH A & B POTASEIUM DIHYDROGEN PHOSPHATE .8g
PH NEEDS TO BE 5.5
 

Lordoftheshard 2

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Could you explain in more depth the complete procedure and things easier to understand for idiots like me
Medium A what it. Consists of
Medium B same as above
Medium C same as above
and the complete procedure whi the how long to leave each medium what temps and so forth and in layman's terms
I'm thankfull for your knowledge a would love to produce my own noreph
 
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azides

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Could you explain in more depth the complete procedure and things easier to understand for idiots like me
Medium A what it. Consists of

If you DONT UNDERSTAND DONT do it.WHile making LPAC is like brewing beer the NEXT STEP


this shit involves CYANIDE and BROMINE TOGETHER to MAKE Cyanogen bromide is TOXIC shit.


Cyanogen Bromide can affect you when breathed in and
by passing through your skin.
* Contact can irritate the skin and eyes.
* Breathing Cyanogen Bromide can irritate the nose and
throat.
* Breathing Cyanogen Bromide may irritate the lungs
causing coughing and/or shortness of breath. Higher
exposures can cause a build-up of fluid in the lungs
(pulmonary edema), a medical emergency, with severe
shortness of breath.
* High exposure to Cyanogen Bromide can cause fatal
Cyanide poisoning with flushing of the face, chest
tightness, headache, nausea, vomiting, weakness,
confusion, dizziness, and trouble sleeping. High levels
may cause convulsions and death




The well-known reaction of hydrazides with cyanogen bromide, usually performed in the presence of potassium or sodium bicarbonate, affords 2-amino-5-substituted-1,3,4-oxadiazoles. In the past 10 years, this reaction has been applied several times, mainly in order to obtain biologically active derivatives....

My nickname is AZIDES... AZIDES go BOOM ... A hydrazide is converted to the corresponding azide in the presence of an acid and a nitrite. Hydrazoic acid can be made from just azides and an acid (water).

See


How Dangerous Is Too Dangerous? A Perspective on Azide Chemistry


How Dangerous Is Too Dangerous? A Perspective on Azide
Chemistry
Cite This: J. Org. Chem. 2022, 87, 11293−11295 Read Online
ACCESS Metrics & More Article Recommendations
All chemists should be aware of the risks inherent to their
work and should consider how to adequately protect
themselves and their colleagues from such hazards. This begs
the question: Can a reaction be so dangerous that, in a general
purpose laboratory, even in the presence of such precautions,
the residual risk is still too high? We contend that yes, certain
reactions fall into this category: those that employ stoichio-
metric quantities of hydrazoic acid, those that form transition
metal azides, and those that combine inorganic azide with
dichloromethane.
A recent article in this journal authored by Gazvoda et al.
describes a procedure for preparing triazoles from alkynes
using stoichiometric sodium azide, stoichiometric acid, and
catalytic copper, followed by a workup that may include
dichloromethane.1,2 As industrial chemists with decades of
experience safely scaling up azide chemistry, we feel compelled
to share with the research community our three major safety
concerns with this procedure.
In the first case, the combination of sodium azide and acid
affords hydrazoic acid. Hydrazoic acid is both acutely toxic
(mouse LD50 = 22 mg/kg)3 and a powerful explosive; in its
neat form, hydrazoic acid is more explosive than TNT and
orders of magnitude less stable.4 The first scientists to isolate
hydrazoic acid (Curtius and Radenhausen, in 1891)5 found
that “the blast of 50 mg was sufficient to disintegrate the
apparatus to dust” and when a subsequent 700 mg batch
“exploded spontaneously”, it seriously injured the coauthor
(Radenhausen) and the shock wave from the explosion
shattered every glass vessel nearby. There is no safe quantity
when dealing with neat hydrazoic acid.
While dilute hydrazoic acid is safer than the neat compound,
it remains extremely dangerous. In the gas phase, mixtures with
nitrogen containing more than 10% HN3 are explosive.4g In
water, a precise value has not been determined, but it is
generally accepted that solutions of >20 wt % HN3 are
explosive.6 The unique risk posed by hydrazoic acid in solution
is that due to its low boiling point (∼36 °C), inadvertent
evaporation and recondensation of a dilute, nonexplosive
solution can result in a concentrated, explosive solution (see
Figure 1).7 It is critical to understand that condensed droplets
of concentrated hydrazoic acid require neither oxygen nor a
spark in order to explode (i.e., the so-called “fire triangle” does
not apply).4b The slightest amount of friction or impact can
result in detonation. Numerous explosions have been reported
when dealing with hydrazoic acid in solution, many of which
have unfortunately led to injuries and deaths.8
In general, when dilute hydrazoic acid solutions are to be
generated or stored, best practices are to add a low-boiling
solvent (such as ether or pentane) to dilute any vapor and/or
condensate.4f Calculations based on the temperature and pH
may be necessary to understand appropriate safe concentration
limits.6b,7b Additionally, if a reaction system contains hydrazoic
acid or may generate hydrazoic acid, a continuous nitrogen
purge of the headspace may be employed to prevent
condensation, and the entire apparatus may be maintained
above 37 °C to ensure no hydrazoic acid can condense.
Returning to the procedure for triazole synthesis disclosed
by Gazvoda et al., the second major safety concern is the
Published: September 2, 2022
Figure 1. Application of Henry’s Law and Antoine’s Equation to a 2.0
wt % solution of HN3 in water at 25 °C9
Editorialpubs.acs.org/joc
Published 2022 by American Chemical
Society 11293
https://doi.org/10.1021/acs.joc.2c01402
J. Org. Chem. 2022, 87, 11293−11295Downloaded via 73.170.156.34 on January 19, 2024 at 22:51:42 (UTC).See https://pubs.acs.org/sharingguidelines for options on how to legitimately share published articles.
combination of copper salts and sodium azide. There have been
more than a dozen documented explosions stemming from
copper(I) azide, copper(II) azide, or unidentified mixtures of
copper with sodium azide or hydrazoic acid.10 The number of
individuals killed by these explosions is at least 16. There is no
general best practice for adding transition metals to reactions
containing inorganic azide or hydrazoic acid, because such an
act is extremely hazardous. Highly explosive, shock-, friction-,
and static-sensitive azide salts have been prepared from Al, Ca,
Ti, V, Cr, Mn, Co, Ni, Cu, Zn, Mo, Pd, Ag, Cd, Sn, Sb, Te, Ba,
Pt, Au, Hg, Tl, Pb, and Bi.4b Copper(II) azide, in particular,
has been reported to be so shock-sensitive that gently
disturbing the crystalline solid, even under water, leads to a
violent explosion.10b Because of this, industrial facilities that
prepare or use inorganic azides take great pains to ensure that
metals are rigorously excluded (i.e., no metal reactor
components, no metal fittings, no metal thermocouples, no
metal scoops or spatulas; even floor drains are covered to
prevent azide from making its way into copper pipes).4b,e
The last major safety concern encountered in the procedure
from Gazvoda et al. is the use of dichloromethane in the
workup. As has been reported numerous times, the
combination of inorganic azide and dichloromethane can
lead to highly explosive, shock-sensitive diazidomethane. As
with hydrazoic acid and copper azide, this dangerous
compound has been implicated in a number of explosions
including those that have led to serious injuries.11
We would like to close with an earnest reminder to all
laboratory chemists that working with inorganic azide requires
diligence. As a general rule, acids, halogenated solvents, and
metals should be strictly avoided. We further recommend that
both authors and reviewers keep these serious safety concerns
in mind when preparing and evaluating manuscripts. We all
must do our part to spread awareness of extreme hazards to
avoid repeating the tragic mistakes of the past.
Daniel S. Treitler orcid.org/0000-0001-5375-4920
Simon Leung
■ AUTHOR INFORMATION
Complete contact information is available at:
https://pubs.acs.org/10.1021/acs.joc.2c01402
Notes
Views expressed in this editorial are those of the authors and
not necessarily the views of the ACS.
Both authors are employees of Bristol Myers Squibb. Bristol
Myers Squibb participated in the review and approval of this
manuscript.
■ ACKNOWLEDGMENTS
The authors would like to sincerely thank Andrej Shemet and
Vladislav Lisnyak for help with translation of non-English
publications. Additionally, the authors are indebted to Michael
Dummeldinger for assistance with Henry’s Law/Antoine’s
Equation calculations for hydrazoic acid in the vapor phase.
The authors would also like to thank Gregg Feigelson, Lakshmi
Narasimhan, Zachary Garlets, and Trevor Sherwood for their
careful review of the manuscript.
■ REFERENCES
(1) Jankovič , D.; Virant, M.; Gazvoda, M. Copper-Catalyzed Azide-
Alkyne Cycloaddition of Hydrazoic Acid Formed In Situ from Sodium
Azide Affords 4-Monosubstituted-1,2,3-Triazoles. J. Org. Chem. 2022,
87, 4018.
(2) Our communications with professor Gazvoda prompted a
correction to the original publication: Jankovič , D.; Virant, M.;
Gazvoda, M. Correction to “Copper-Catalyzed Azide-Alkyne Cyclo-
addition of Hydrazoic Acid Formed In Situ from Sodium Azide
Affords 4-Monosubstituted-1,2,3-Triazoles”. J. Org. Chem. 2022, 87,
8277.
(3) (a) Trout, D.; Esswein, E. J.; Hales, T.; Brown, K.; Solomon, G.;
Miller, M. Exposures and health effects: an evaluation of workers at a
sodium azide production plant. Am. J. Ind. Med. 1996, 30, 343. (b)
Lewis, R. J., Sr., Ed. Sax’s Dangerous Properties of Industrial Materials;
Wiley & Sons, Inc.: Hoboken, 2004.
(4) (a) Fedoroff, B. T.; Aaronson, H. A.; Sheffield, O. E.; Reese, E.
F.; Clift, G. D. Encyclopedia of Explosives and Related Items; Picatinny
Arsenal: Dover, 1960. (b) Fair, H. D., Walker, R. F., Ed. Energetic
Materials Vol 1: Physics and Chemistry of the Inorganic Azides; Plenum
Press: New York, 1977. (c) Pepekin, V. I. Detonation parameter
criterion for explosives. Polym. J. Chem. 1981, 55, 1405. (d) Patnaik,
P. A Comprehensive Guide to the Hazardous Properties of Chemical
Substances; Van Nostrand Reinhold, 1992. (e) Peer, M. Dangerous
reactions. Sodium azide in industrial organic synthesis. Informations
Chimie. 1997, 98. (f) Urben, P. G., Ed. Bretherick’s Handbook of
Reactive Chemical Hazards; Academic Press: Boston, 2007. (g) Wiss,
J.; Fleury, C.; Heuberger, C.; Onken, U. Explosion and Decom-
position Characteristics of Hydrazoic Acid in the Gas Phase. Org.
Process Res. Dev. 2007, 11, 1096.
(5) Curtius, T.; Radenhausen, R. For Knowledge about the
Hydrogen Azide. J. Prakt. Chem. 1891, 43, 207.
(6) (a) Kurbangalina, R. K.; Patskov, E. A.; Stesik, L. N.; Yakovleva,
G. S. Detonation of liquid hydrazoic acid and its aqueous solutions.
Prikladnaya Mekhanika i Tekhnicheskaya Fizika 1970, 160. (b) Ertel,
D.; Schmieder, H.; Stollenwerk, A. H. The behavior of hydrazoic acid
in PUREX process solutions under safety aspects. Nukleare Entsorgung
1989, 107. (c) Ullman’s Encyclopedia of Industrial Chemistry; VCH:
New York, 1989; Vol. A13 “Hydrazoic Acid and Azides”.
(7) (a) Betterton, E. A.; Robinson, J. L. Henry’s Law Coefficient of
Hydrazoic Acid. J. Air Waste Manage. Assoc. 1997, 47, 1216.
(b) González-Bobes, F.; Kopp, N.; Li, L.; Deerberg, J.; Sharma, P.;
Leung, S.; Davies, M.; Bush, J.; Hamm, J.; Hrytsak, M. Scale-up of
Azide Chemistry: A Case Study. Org. Process Res. Dev. 2012, 16, 2051.
(c) Treitler, D. S.; Leung, S.; Lindrud, M. Development and
Demonstration of a Safer Protocol for the Synthesis of 5-
Aryltetrazoles from Aryl Nitriles. Org. Process Res. Dev. 2017, 21, 460.
(8) (a) Curtius, T. Abstracts: On hydrazoic acid (azoimide). J. Am.
Chem. Soc. 1890, 12, 472. (b) Browne, A. W.; Lundell, G. E. F.
Anhydrous hydronitric acid. I. Electrolysis of a solution of potassium
trinitride in hydronitric acid. J. Am. Chem. Soc. 1909, 31, 435.
(c) Cooper-Key, A.; Crozier, T. H.; Thomas, R. A.; Watts, H. E.;
Malcolm, C. R. Fiftieth Annual Report of His Majesty’s Inspectors of
Explosives; His Majesty’s Stationary Office: London, 1926. (d) Sha-
piro, E. L. Hydrazoic acid explosion. Chemical & Engineering News
(Bloomfield, NJ) 1974, No. Jan, 14. (e) Sood, R. K.; Nya, A. E. Short
note on non-explosive distillation of HN3. J. Therm. Anal. 1981, 20,
491. (f) United States Department of Labor Occupational Safety and
Health Administration. Accident: 699603 - Employee Killed in Drum
Explosion. Inspection #102595436. Event Date October 7 1995.
https://www.osha.gov/pls/imis/accidentsearch.accident_detail?id=
699603 (accessed 2022-05-27). (g) Crabbe, N. Glass embedded in
student’s abdomen in lab explosion. Gainesville Sun (Gainesville, FL)
2012, January 18 https://www.gainesville.com/story/sports/college/
2012/01/18/glass-embedded-in-students-chest-abdomen-in-lab-
explosion/64271845007/ (accessed 2022-05-27). (h) Taton, T. A.;
Partlo, W. E. Chemical Safety: Explosion hazard in synthesis of
azidotrimethylsilaneChemical & Engineering News (Twin Cities, MN)
2014, October 27.
(9) Note: This photo was staged for demonstration purposes; the
flask does not actually contain a hydrazoic acid solution.
The Journal of Organic Chemistry pubs.acs.org/joc Editorial
https://doi.org/10.1021/acs.joc.2c01402
J. Org. Chem. 2022, 87, 11293−11295
11294
(10) (a) Dennis, L. M.; Isham, H. Hydronitric Acid, V. J. Am. Chem.
Soc. 1907, 29, 18. (b) Turrentine, J. W. Contributions to the
Electrochemistry of hydronitric acid and its salts. I. The corrosion of
some metals in sodium trinitride solution. J. Am. Chem. Soc. 1911, 33,
803. (c) Hitch, A. R. Thermal decomposition of certain inorganic
trinitrides. J. Am. Chem. Soc. 1918, 40, 1195. (d) Cirulis, A. Copper
azide and its complexes. Naturwissenschaften 1939, 27, 583. (e) Cirulis,
A. The explosive properties of Cu(N3)2. Zeitschrift fuer das Gesamte
Sciess- und Sprengstoffwesen 1943, 38, 42. (f) Becher, H. H. Use of
sodium azide is dangerous. Naturwissenschaften 1970, 57, 671.
(g) Kabik, I.; Urman, S. Hazards of copper azide in fuzes. In
Proceedings of Minutes of the 14th Explosive Safety Seminar, New
Orleans, Louisiana − Department of the Defense Explosive Safety Board,
1973. (h) Cowely, B. R.; Oughton, J. F. Detonation of heavy metal
azides. Chemistry & Industry 1973, 444. (i) Wear, J. O. CXX. Azide
Hazards with Automatic Blood Cell Counters. Journal of Chemical
Education (Safety in the Chemical Laboratory Supplement) 1975, 52,
A23. (j) Pobiner, H. Chemical Safety: Hazard with sodium azide.
Chemical & Engineering News (Princeton, NJ) 1982, No. April, 12.
(k) Bentur, Y.; Koren, G.; McGuigan, M.; Spielberg, S. P. An unusual
skin exposure to copper; clinical and pharmacokinetic evaluation.
Journal of Toxicology: Clinical Toxicology 1988, 26, 371. (l) Sood, R.
K.; Alobi, N. O. Cupric Azide - A New Detonator for Mining. Global
Journal of Pure & Applied Sciences 1997, 3, 69. (m) Mortar Accident
Mali; Dutch Safety Board: The Hague, 2017.
(11) (a) Bretherick, L. Azide-halosolvent hazards. Chemical &
Engineering News (Dorset, UK) 1986, No. December, 22. (b) Peet, N.
P.; Weintraub, P. M. Explosion with sodium azide in DMSO-CH2Cl2.
Chemical & Engineering News (Cincinatti, OH) 1993, No. April, 19.
(c) Hruby, V. J.; Boteju, L.; Li, G. Chemical Safety: Explosion with
sodium azide. Chemical & Engineering News (Tucson, AZ) 1993,
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explosion. Org. Process Res. Dev. 2008, 12, 1285.
The Journal of Organic Chemistry pubs.acs.org/joc Editorial
https://doi.org/10.1021/acs.joc.2c01402
J. Org. Chem. 2022, 87, 11293−11295
11295

Now then did any of this make sense? DO you uunderstand the dangers. IF not this route is not for the avg bee.
 
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azides

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https://www.science.org/content/blog-post/things-i-won-t-work-cyanogen-azide


Cyanogen bromide is not a nice reagent. It’s not quite on my list of things that I refuse to use, but it’s definitely well up on the list of the ones I’d rather find an alternative to. The stuff is very toxic and very volatile, and reactive as can be.
But it’s not the worst thing in its family. A good candidate for that would be cyanogen azide, which you get by reacting the bromide with good old sodium azide. Good old sodium azide, which is no mean poison itself, will do that with just about any bromide that’s capable of being displaced at all. Azide is one of the Nucleophiles of the Gods, like thiolate anions – if your leaving group doesn’t leave when those things barge in, you need to adjust your thoughts about it. Cyanogen bromide (or chloride) doesn't stand a chance. Marsh's papers are, most appropriately, well marbled with warnings about how to handle the stuff. It's described as "a colorless oil which detonates with great violence when subjected to mild mechanical, thermal, or electrical shock", and apologies are made for the fact that most of its properties have been determined in dilute solution. For example, its boiling point, the 1972 paper notes dryly, has not been determined. (The person who determined it would have to communicate the data from the afterworld, for one thing). The experimental section notes several things that the careless researcher might not have thought about. For one thing, you don't want to make more than a 5% solution in nonpolar solvents. Anything higher and you run the risk of having the pure stuff suddenly come out of solution and oil out on the bottom of the flask, and you certainly don't want that. You also don't want to make a solution in anything that's significantly more volatile than the azide, because then the solvent can evaporate on you, making a more concentrated stock below, and you don't want that, either

Alternatively, follow the “rule of six:” six carbons (or other atoms of about the same size) per energetic functional group (azide, diazo, nitro, etc.) should provide enough dilution to render the compound relatively safe to work with given appropriate controls and safety procedures.


In general, olefinic, aromatic, or carbonyl azides are much less stable than aliphatic azides.

Broadly speaking, therefore, the acid hydrazide and cyanogen halide are simply contacted by being mixed together in solution. Cyanogen bromide..




ThePhantom1994
3y ago

Put that thing back where it came from or so help me


deleted]
3y ago

Made by reacting Cyanogen Chloride or Cyanogen Bromide with Sodium Azide in Acetonitrile


Direwolf202

3y ago

Can we go a step further in putting it back where it came from please. The resulting mixture of Sodium, Chlorine, and Bromine isn't too nice - but it's better than those!

https://www.reddit.com/r/cursed_chemistry/comments/lcglnk
If you are asking Could you explain in more depth the complete procedure and things easier to understand for idiots like me

Medium A what it. Consists of I ask you to not WALK BUT RUN AWAY if you don't understand what is happening

Remember A hydrazide is converted to the corresponding azide in the presence of an acid and a nitrite. Hydrazoic acid can be made from just azides and an acid (water). IF you don't know what the FUCK you are doing... RUN away.
 

azides

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Sodium azide (NaN3) looks like common table salt. But it kills everything from bacteria and fungi to mammals - including humans. It is as powerful a poison as sodium cyanide.

As a graduate student, Betterton learned first-hand that even a whiff of hydrazoic acid (HN3) -- sodium azide's conjugate acid - can be dangerous. While conducting a laboratory experiment with the dangerous compound, he suddenly felt dizzy, his blood pressure dropped, his heart raced and his eyes flushed bloodshot red.

Eating as little as 50 milligrams (less than two-thousandths of an ounce) of sodium azide can lead to collapse and a coma-like state within five minutes as blood pressure plummets and heart rate skyrockets. Ingest a few grams, and death occurs within 40 minutes.. What is known is that sodium azide is water-soluable. "Spills therefore could potentially migrate into sewers, streams, lakes, and groundwater systems," Betterton said. The compound easily pronates (adds a proton) when wet, becoming volatile hydrazoic acid, a potential threat to sanitation workers, for example, he added.

Azide is one of the Nucleophiles of the Gods, like thiolate anions – if your leaving group doesn’t leave when those things barge in, you need to adjust your thoughts about it. This can not be understated enough Remember A hydrazide is converted to the corresponding azide in the presence of an acid and a nitrite. Hydrazoic acid can be made from just azides and an acid (water). The compound easily pronates (adds a proton) when wet, becoming volatile hydrazoic acid IF you don't know what the FUCK you are doing... RUN away. hydrazoic acid shows some analogy to the halogen acids, since it forms poorly soluble (in water) lead, silver and mercury(I) salts. The metallic salts all crystallize in the anhydrous form and decompose on heating, leaving a residue of the pure metal.

in its neat form, hydrazoic acid is more explosive than TNT and orders of magnitude less stable. Let me tell you how unstable azides are. SHAKE SHAKE sodium azides... dumb move... it go boom.Metal spoon it go boom. hydrazoic acid made from just water and an azide go boom from from the garbage truck rumbling outside....


this is like chem 101 lesson if you ever decide to fuck with azides.

when you mess around with turning a phenol (like calmus oil or bitter almond oil ie benzaldehyde into an azide ... and you mixed solvent, bromo coumpound AND AN AZIDE...

Still


TIMED IGNITION OF EXPLOSIVES AND FLAMMABLES FROM DESENSITIZED SOLUTIONS Author(s) Gerstein, M; Choudhury, PR Year 1984 Publisher AIAA Location New York, NY, USA Volume 95

https://hero.epa.gov/hero/index.cfm/reference/details/reference_id/8352607

Abstract This paper is concerned with the EVAPORATION of SINGLE DROPS of binary mixtures composed of an explosive solute in a solvent (ammonium azide in water and ozone in liquid oxygen) and a spontaneous flammable solute (white phosphorus) in carbon disulphide (in this case white phosphorus was probably subbed for the almost just as dangerous potassium nitrate (KNO3), potassium nitrate It is used to make explosives, matches, fertilizer, fireworks, glass and rocket fuel.

. The equations are general and may be applied to more complex systems (ie subbing phosphours for (KNO3) IS JUST AS BAD... of course airbags are the examplein this case.. The work is easily expanded to groups of drops to simulate a spray and to sprays if a distribution function is known.

Anyways I might not know shit for shit about hydrazoic acid but

miket928

21d ago

This is partially correct but largely out of context. A more likely scenario is that whatever material encases the azides in the airbag was compromised, allowing water to enter. Acidification of sodium azide in water produces hydrazoic acid, which has a low boiling point and is highly shock-sensitive and explosive. If hydrazoic acid formed upon exposure to water, and then evaporated and condensed onto another surface, then you essentially have a bomb that was set off by the vibration of the garbage truck. I'll note that this is also speculative, but it makes more sense to me than the chemistry cited in the lengthy reply above.
The general theme of the reply is correct though - azides are not to be fucked with. Not only are they potentially explosive, but they are also highly toxic.
Source: I have a PhD in chemistry. (And I can recall a time when a building was evacuated and the bomb squad was called in to dispose of an unclaimed flask in a cold room that contained clear liquid labeled HN3 (hydrazoic acid).)

https://www.reddit.com/r/Detailing/comments/18t8u8e/_/kfgwzlm
 

azides

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In my head while people may have done it in the past I sure as shit hope people knew what they are doing. Or I misreading this and there is nothing to fear... eitherway, the careless researcher shouldn't even work with cyanogen azide, or Cyanogen Bromide or anything like it, but you never can tell what fools will get up to. The compound has around a hundred references in the literature, a good percentage of which are theoretical and computational. Most of the others are physical chemistry, studying its decomposition and reactive properties. You do run into a few papers that actually use it as a reagent in synthesis, but I believe that those can be counted on the fingers, which is a good opportunity to remind oneself why they're all still attached.
https://www.science.org/content/blog-post/things-i-won-t-work-cyanogen-azide

I
imagine someone wreck less they aren't avoiding water and strong acids which can lead to the formation of hydrazoic acid, which is highly toxic, volatile, and explosive. But you know I'm just thinking out loud...
 

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I see this is cis vs trans... Either way one shouldn't fuck with cyanide salts unless you understand...
 

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Does this method also work for halostachine and 3-methyl aminorex?
 

situ1984

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Can this method be replaced with ephedrine?
 

btcboss2022

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Ok thats racemic one thanks a lot, isomer resolution of 4-MAR I guess could be made as usual any option?
Thanks.
 

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More clarification on the 4-MAR w/out CNBr route


SPISSHAK Epimeriztion of optically active compds.

see Patent US2214034 for an alternative. This is because of aziridine formation during HCl reflux.


You mention racemiztion of ppa with HCl I don`t recommend this see Patent US2214034 for an alternative. This is because of aziridine formation during HCl reflux.

This patent will provide a method which according to the aurthor, The hydrogen gas liberatied during racemization serves to protect the ephedrines from decomposition.
 

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These may have been posted already,sorry bout` that.
Some may find the reading fun.

Patent EP1142864

An efficient process for stereoselectively producing L-erythro-(1R,2S)-2-amino-1-phenylpropan-1-ol from L-(R)-phenylacetylcarbinol, which comprises reductively aminating L-(R)-phenylacetylcarbinol with a primary aralkylamine under catalytic reduction conditions and successively subjecting the resultant L-erythro-(1R,2S)-2-(N-aralkylamino)-1-phenylpropan-1-ol to catalytic reduction to remove the N-aralkyl group in a manner as in hydrogenolysis.

Patent GB365535

I-Phenyl-2-aminoalcohols-(1); oximes.--l-1-Phenyl-2-aminopropanols-(1) are prepared by (1) treating l-1-phenyl-2-ketopropanol-(1) with hydrogen and either (a) a precious metal catalyst in presence of ammonia or a primary or secondary amine excepting methylamine, or (b) a catalyst comprising iron, cobalt, nickel or copper in the presence of an ammonium salt or a salt of a primary or secondary amine; (2) converting l-1-phenyl-2-ketopropanol-(1) into its oxime with hydroxylamine and catalytically reducing it with a precious metal catalyst. The product of (2) may be alkylated to yield the corresponding alkylamino compound. Examples are given of the preparation of (1) l-1-phenyl-2-aminopropanol-(1) by treating l-phenylacetylcarbinol with hydroxylamine and hydrogenating the resulting oxime in acetic acid solution using palladium as catalyst, and (2) l-1-phenyl-2-methylaminopropanol-(1) by the hydrogenation of a solution of l-phenylacetylcarbinol and methylamine hydrochloride in alcohol in the presence of nickel. Specification 313,617 is referred to. The Provisional Specification describes also the conversion of optically active 1-phenyl-2-ketoalcohols in general into the corresponding 1-phenyl-2-aminoalcohols-(1) by the foregoing processes, and includes an example of the hydrogenation of l-phenylacetylcarbinol in alcohol solution in presence of methylamine using palladium as catalyst to form l-phenylpropanolmethylamine.

Patent GB365541

1 - Phenyl-2-aminoalcohols - (1).--Racemic 1-phenyl-2-aminopropanols-(1) are prepared by treating l-1-phenyl-2-ketopropanol-(1) with hydrogen in presence of ammonia or a primary or secondary amine using iron, nickel, cobalt, or copper as the catalyst. An example is given of the conversion of l-phenylacetylcarbinol into racemic 1-phenyl-2-methylaminopropanol-(1) by hydrogenation in the presence of methylamine and nickel. Specification 313,617, [Class 2 (iii), Dyes &c.], is referred to. The Provisional Specification describes also the conversion of optically active 1-phenyl-2-ketoalcohols-(1) in general into the corresponding 1-phenyl-2-aminoalcohols-(1) in the racemic form by the foregoing process.

Patent US4224246

A process for the synthesis and separation of the threo and erythro isomers of 2-amino-1-phenyl-1-propanol comprising the steps of catalytically reducing 2-nitro-1-phenyl-1-propanol to form the acetate salt of the racemic mixture of 2-amino-1-phenyl-1-propanol and separating the isomers by fractional crystallization.


The reaction mixture of reduced nitro alcohols was resolved into optically pure isomers by the following process.

A mixture of a DL-threo-2-amino-1-phenylpropanol (1 mole) in dichloromethane (600 ml.), dibenzoyltartaric acid (0.5 mole) in distilled water (30 ml.), and sodium hydroxide (0.5 mole) in distilled water (50 ml.) is stirred rapidly for two hours and allowed to stand for two hours. The dichloromethane phase is separated using a separating funnel over anhydrous magnesium sulfate. Rotary evaporation of the dichloromethane phase gives the L-threo isomer in nearly quantitative yield.

The aqueous phase is made alkaline with ammonia to pH 13 and extracted with dichloromethane. The dichloromethane extract is dried over anhydrous magnesium sulfate and evaporated to give the D-threo isomer in nearly quantitative yield. The enantiomeric purity of the products is 96-99% based on GLC analysis of the D or L-
000438325-file_lwwo.gif
-methoxy-
000438325-file_lwwo.gif
-trifluromethylphenylacetamide (MTPA) derivatives.
 
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