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Chemi Pharma
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Quote: Originally posted by FireLion3  | | You said you were in Latin America? Are the regulations strict there? In the US there's not that many chemicals that require filling out a bunch of
paperwork to get, unless someone is trying to purchase known precursor chemicals, or purchasing ridiculous quantities of watched chemicals. For the
most part the US chemical market is pretty open. At least in my opinion. I know other countries out there are far more regulated, especially in
Europe. |
Here in Brazil we have three kind of regulations: The first one is dicted by Army Forces and control the chemical weapons precursors. Private persons
can by only 02 kgs at maximum, filling papers and attaching their documents, explaining why they have a legitimate use to that chemical.
The second one is dicted by Federal Police Department (our FBI) and control the maximum quantities of chemicals that are common employed as precursors
of narcotics manufactory. Private persons can purchase monthly a few quantities without a special licence required.
The third one is dicted by the public health autorities (here called ANVISA), and restrict the commerce and manufacturing of legal psichoative
chemical compounds. License is always required. The bureau also maintain a monthly list containing the banned drugs, alkaloids and narcotics for
criminal law enforcement use.
The most of chemical reagents is free to purchase without restrictions and you can do that easily at chemical supliers or even on the NET. I know that
many other countries like Australia get almost anything under strict control. southern Asia too. East european countries as far as I know have the
most liberal rules worldwide.
May be would be interesting to create a thread about the chemical restrictions existing nowadays in every country, just for fun.
[Edited on 25-2-2018 by Chemi Pharma]
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DrDevice
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ChemiPharm wrote (a long time ago now)
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I found that Liebig have synthesized and discovered cyanuric chloride in 1827, by passing chlorine into a flask with dry potassium thiocyanate, what
seems not too difficult. However, I found nowhere on the NET this synthesis in details. If anybody here could get it and post here, it will be much
appreciated.
The industrial way to make it reacting Chlorine with HCN is far from what can be made by an amateur chemist without risk of death.
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I think I have tracked down the original article. I don't speak German, and haven't Google translated yet, but there is a mention of
"Schwefelcyankaliums" which translates to "sulfur cyanide potassium".
Attachment: liebig1829.pdf (1.2MB)
This file has been downloaded 455 times
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woelen
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Schwefelcyankalium stands for potassium sulfocyanide. In modern nomenclature this is potassium thiocyanate, KSCN.
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DrDevice
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I've had a go at translating the first few paragraphs. Had to tweak the OCR results a few times, and I hope the German speakers forgive for not
keeping the umlauts.
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Schwefelcyankalium und Chlor.
Schmilzt man trocknes Schwefelcyankalium in einem Strom von trocknem Chlorgas, so blaht sich dieses SaIz heftig auf, wird gelb
und undurchsichtig, seine Flussigkeit verliert sich immer mehr, nach Maafgabe als dic Zersetzung vorwarts schreitet, bis dafs es zuletzt fest wird; es
destillirt wie bei den vorhergehenden Zersetzungen Chlorschwefel und Chlorcyan uber; allein in einem gewissen Zeitpunkte erhebt sich ein dicker rother
Dampf, der sich an dem oberen Theil des Gefafses in Gestalt einer rothen, an manchen Stellen gelbrothen Masse anlegt.
Sie lafst sich in Gestalt von Blattchen, die keine Spur von Krystallisation zeigen, von dem Gefafse ablosen, und besitzt einen starken Geruch nach
Chlorcyan, der sich aber beiin Erhitzen an der Luft verliert. Sie ist im Wasser unaufloslich und wird von Sauren, aufser Salpetersaure, nicht
zersetzt; in Vitriolol lost sie sich auf, wird aber beim Verdunnen wieder abgeschieden. Die verschieden gefarbten Stellen scheinen darauf hinzudeuten,
dafs diese Substanz zwei verschiedene feste Verbindungen enthalt; dies bestatigt auch ihr Verhalten zum Aetzkali.
Uebergeifst man namlich diese Substanz feingepulvert mit Aetzkali, so farbt sie sich dunkelroth, und das Kali lost nichts oder nur wenig davon auf;
giefst man die alkalische Flussigkeit ab, und spult den Ruckstand mit etwas Weingeist ab, so lost er sich alsdann beim Uebergiefsen mit reinem Wasser
zum Theil auf, wahrend ein anderer Theil, ohne Zweifel eine hohere Schwefelungsstufe, in Gestalt von gelben Flocken zuruckbleibt.
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This translates to:
Potassium thiocyante and chlorine.
If you melt dry potassium thiocyanate in a stream of dry chlorine gas, this salt inflates violently and turns yellow
and opaque, its fluidity loses itself more and more, according to the measure as the decomposition proceeds until it finally becomes solid; chlorine
sulfur and cyanogen chloride distill over, as in the previous decompositions; only at a certain point in time does a thick red vapor rise, which forms
a red, yellow-red mass in some places on the upper part of the vessel.
It can be in the form of leaves, which none show traces of crystallization, detach from the vessels and has a strong smell of cyanogen chloride, which
is lost in the air when heated. It is insoluble in the water and is acidic, as well as Nitric acid, not decomposed; it dissolves in Vitriolol, but is
deposited again when thinning. The different colored areas seem to indicate that this substance is two different solid connections contains; this also
confirms their attitude towards Aetzkali.
This substance is finely powdered with aetzkali, it turns dark red, and the potash dissolves none or little of it; you pour off the alkaline liquid
and rewind the a little spirit, then it partially dissolves when pouring over with pure water, while a other part, no doubt a higher level of
sulfurization, remains in the form of yellow flakes.
___________
Following this is a series of description of characterisation experiments. A little later in the document though we get to:
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Der gelbe Korper lafst sich ebenfalls und viel sicherer und vortheilhafter darstellen, wenn man Chlorgas durch eine concentrirte Auflosung von
Schwefelcyankalium leitet.
Sogleich, wenn die ersten Blasen Chlorgas in diese Auflosung treten, bildet sich ein gelber Niederschlag, der bestandig zunimmt; dies geschieht aber
nur dann, wenn das Schwefelcyankalium- kein kohlensaures Kali enthalt, welches nach der gewohnlichen Methode, wenn man Weingeist zur Scheidung beider
anwendet, Ieicht geschicht. Man verfahrt deshalb bei der Darstellung des Schwefelcyankaliums besser, wenn man, nach dem das Eisencyankalium mit
Schwefel zusammengeschmolzen und im Wasser wieder aufgelost ist, das Eisenoxydul zum Theil mit kohlensaurem Kali, und nachber vollstandig mit
Schwefelammonium fallt, die Flussigkeit abdampft und bis zur vollstandigen Zersetzung des Schwefelcyanammoniums schmilzt;
Der gelbe Niederschlag backt bei dem Trocknen stark zusammen, er fuhlt sich weich an und farbt sehr stark ab, er halt das Wasser beim Trocknen
aufserst hartnackig zuruck. Sein Verhalten stimmt so genau mit dem der beschriebenen Schwefelcyanverbindungen uberein,
dafs man beide schon darnach fur identisch zu halten geneigt ist.
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This translates as:
The yellow body can also be displayed much more safely and favorably if you pass through chlorine gas conducts a concentrated solution of potassium
thiocyanate.
Immediately when the first bubbles of chlorine gas enter this solution, a yellow precipitate forms steadily increases; however, this only happens if
the potassium thiocyanate - contains no potassium carbonate, which according to the usual method, if one uses wine spirit to separate the two, is easy
to tell. It is therefore better to proceed with the representation of the cyanide of sulfur if one follows the cyanide of iron with Sulfur melted
together and in the water again the iron oxide is partly dissolved with carbon dioxide Potash, and afterwards completely covered with sulfur ammonium,
the liquid evaporates and melts until the sulfur cyanammonium has completely decomposed
The yellow precipitate bakes on drying strong together, it feels soft and colors a lot strong, it keeps the water dry when drying stubbornly back. Its
behavior agrees so exactly that of the sulfur cyanide compounds described, that both are inclined to be considered identical afterwards.
So there is some archaic (?) technical German in there that Google struggles with, and some funky English in the translation, but you get the gist.
When you read things like "the smell of cyanogen chloride" you get a bit worried that the first procedure might be hazardous to one's health (more so
than usual...)
Passing the chlorine into a saturate potassium thiocyanate solution seems to do something however. Cyanuric chloride though reacts with water - maybe
not quickly and it can be filtered and dried?
Brave souls who regularly use chlorine might want to give this a go??
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Mush
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Reaction of Carboxylic Acids with Sulfur Monochloride Using Iodine as Catalyst
Yoshiyuki TAKADA, Toshio MATSUDA, Hotuma OKASAKA
1969 Volume 72 Issue 11 Pages 2502-2503
https://doi.org/10.1246/nikkashi1898.72.11_2502
Attachment: 1969 Volume 72 Issue 11 Pages 2502-2503.pdf (540kB)
This file has been downloaded 397 times
3) V. Auger, A. Behal, Bull. soc. chim., [ 3 ] 2. 44 (1889). -> 144
Originally posted at the hive
" OTC acetyl chloride"
https://the-hive.archive.erowid.org/forum/showflat/Cat-/Numb...
SCl2 and SOCl3 are generated in situ:
S + Cl2 -> SCl2
CH3-COOH + SCl2 + Cl2 -> CH3-COCl + SOCl3 + HCl
CH3-COOH + SOCl3 -> CH3-COCl + SO2 + HCl
V.Auger, A.Behal, Bl. (3) 2, 145 (1889)
Bl =Bull. soc. chim or Bull.
and Houben-Weyl VIII, p.475
Full title:
No 98. — Sur une nouvelle méthode de préparation du chlorure
d'acétyle et de l'acide monochloracetique; par V. AUGER et
A. BÉHAL
 
Machine traslation of part 1. acetyl chloride:
"1. Acetyl chloride. - Sulfur tetrachloride SCI "reacts
on acetic acid according to the equation:
SCl4+ 2CH3COOH = SO2 + 2HCl + 2CH3COCl.
Here is how we operate:
We put in a balloon 1 molecule of sulfur or protochloride
of sulfur, and 2 molecules of crystallizable acetic acid. We do
pass a stream of chlorine through the mixture while cooling the
balloon in a mixture of ice and salt. When chlorine is not
more absorbed, the flask is allowed to return slowly to room temperature, then it is distilled with a very good condenser and
collects the product in a balloon surrounded by ice.
Torrents of hydrochloric acid and sulphurous acid are given off, which always entail a notable quantity of chloride
acid. The liquid which distils before 60 ° is rectified, then it is freed from the sulphurous product which it contains, by stirring it with mercury,
or better still, with copper powder. It then passes pure to distillation.
The yield thus obtained has always been quite low: 500 gr.
of chloride per 600 grams of acid; but it is to think that
by the use of more vigorous refrigeration, such as
coils surrounded by ice, we would increase the efficiency
in notable proportions."
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Cou
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Using TCCA and triphenylphosphine requires column chromatography to purify the products, gross.
Oxalyl chloride is the only reagent I can get for conversion of carboxylic acids to acid chlorides. Unfortunately it's very expensive.
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karlos³
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You should still get it, who knows how long you will be able to access that?
When I got that stuff the first time for myself, I had to drive through the half country(luckily its tiny compared to america) to pick it up because
shipping by mail wasn't legally allowed.
I still did it, because it is just so valuable.
It is also one of the least nastiest and cleanest reagents for acid chlorination, unlike thionyl chloride which I think is worse(although I could get
that shipped by mail), so I can only recommed to buy it.
Yes its not cheap, but ask yourself, is it worth it?
I mean, I don't know about what a price you are talking but I'm sure it will still be worth to get such an useful reagent.
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draculic acid69
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| Quote: Originally posted by Magpie | RCOOH + SOCl2 → RCOCl + SO2 + HCl
SOCl2, thionyl chloride, can be made at home, with much labor. See my "preparation of thionyl chloride," this forum. But SOCl2 is a "3B chemical
weapons" precursor. But, then again, so is PCl3. http://www.australiagroup.net/en/precursors.html
I don't think there is a cheap and easy way to make acid chlorides if that is what you are asking. If it was many here would be doing same. It is
easier to make phosphorus.
[Edited on 21-2-2018 by Magpie] |
In the AA sticky there's info on using sicl4 +GAA---> AA
This is easier to make than socl2+legal+ not sure to buy
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draculic acid69
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| Quote: Originally posted by Mush | Reaction of Carboxylic Acids with Sulfur Monochloride Using Iodine as Catalyst
Yoshiyuki TAKADA, Toshio MATSUDA, Hotuma OKASAKA
1969 Volume 72 Issue 11 Pages 2502-2503
https://doi.org/10.1246/nikkashi1898.72.11_2502
3) V. Auger, A. Behal, Bull. soc. chim., [ 3 ] 2. 44 (1889). -> 144
Originally posted at the hive
" OTC acetyl chloride"
https://the-hive.archive.erowid.org/forum/showflat/Cat-/Numb...
SCl2 and SOCl3 are generated in situ:
S + Cl2 -> SCl2
CH3-COOH + SCl2 + Cl2 -> CH3-COCl + SOCl3 + HCl
CH3-COOH + SOCl3 -> CH3-COCl + SO2 + HCl
V.Auger, A.Behal, Bl. (3) 2, 145 (1889)
Bl =Bull. soc. chim or Bull.
and Houben-Weyl VIII, p.475
Full title:
No 98. — Sur une nouvelle méthode de préparation du chlorure
d'acétyle et de l'acide monochloracetique; par V. AUGER et
A. BÉHAL
Machine traslation of part 1. acetyl chloride:
"1. Acetyl chloride. - Sulfur tetrachloride SCI "reacts
on acetic acid according to the equation:
SCl4+ 2CH3COOH = SO2 + 2HCl + 2CH3COCl.
Here is how we operate:
We put in a balloon 1 molecule of sulfur or protochloride
of sulfur, and 2 molecules of crystallizable acetic acid. We do
pass a stream of chlorine through the mixture while cooling the
balloon in a mixture of ice and salt. When chlorine is not
more absorbed, the flask is allowed to return slowly to room temperature, then it is distilled with a very good condenser and
collects the product in a balloon surrounded by ice.
Torrents of hydrochloric acid and sulphurous acid are given off, which always entail a notable quantity of chloride
acid. The liquid which distils before 60 ° is rectified, then it is freed from the sulphurous product which it contains, by stirring it with mercury,
or better still, with copper powder. It then passes pure to distillation.
The yield thus obtained has always been quite low: 500 gr.
of chloride per 600 grams of acid; but it is to think that
by the use of more vigorous refrigeration, such as
coils surrounded by ice, we would increase the efficiency
in notable proportions."
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I always wondered why ppl weren't trying to use sulphur in situ like with red P.
If it works that's the way for sure.will it also work for benzoic and propionic acid?
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Mush
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| Quote: Originally posted by draculic acid69 |
I always wondered why ppl weren't trying to use sulphur in situ like with red P.
If it works that's the way for sure.will it also work for benzoic and propionic acid?
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RESEARCHES ON HYDANTOINS. SYNTHESIS OF THE
SOPORIFIC, 4,4-PHENYLETHYL-HYDANTOIN(NIRVANOL)
BY WILLIAM T. READ 1922
Preparation of Propionyl Chloride, CsH5COC1.-Propionyl chloride
was prepared not only by the usual methods with phosphorus trichloride
or phosphorus pentachloride, but also by the chlorination of propionic.
acid in the cold with sulfur monochloride present.
To 540 g. of propionic acid 245 g. of sulfur monochloride was added and chlorine was passed through the mixture while it was stirred for 15 hours. The
chlorination proved to be incomplete at this point, since 150 g. of unchanged propionic acid was recovered. There was also considerable sulfur
monochloride, which was removed from
the propionyl chloride by treatment with hydrogen sulfide. The propionyl chloride obtained amounted to 250 g. This product functioned as
satisfactorily in the subsequent preparation of phenylethyl ketone as that prepared by the phosphorus halide methods.28*.
Preparation of aliphatic acid chlorides
US1805162A
A mixture of 120 grams glacial acetic
acid, 100 grams S2Cl2 and 2 grams iron
filings was cooled to —19° C, and 9 oz.
chlorine passed in. keeping the temperature
below -4° C. The reaction mixture was
allowed to stand at 0° C. for 10 hours, and
then fractionally distilled. Yield 150
grams acetyl chloride amounting to 95.5
per cent, of theory.
Similarly, i may prepare the acid chlo-
rides of propionic, butyric, valeric and
homologous aliphatic acids, as well is of
their substitution products, such as the halo-
gen substituted derivatives thereof.
[Edited on 8-10-2020 by Mush]
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Pumukli
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In theory the reaction should work with benzoic acid too. I think that solubility issues would arise though...
The issue with HCl gas could be prevented if one could use the alkali-salt of the acids. Unfortunately the same solubility problems are obvious in
this case as well.
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garphield
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isn't there a thread on here somewhere where someone converted sodium acetate to acetyl chloride using sulfur chlorides? probably won't work with
everything but sulfur and chlorine are very easy to get and sulfur chlorides can be generated from molten sulfur and chlorine gas very easily,
especially compared to thionyl chloride or phosphourus halides.
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clearly_not_atara
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I wonder if you could oxidise sulfur with KICl4? It's a lot easier to deal with than liquid bromine. Particularly so if KICl4 will dissolve in GAA.
4 KICl4 + 3 S + 6 AcOH >> 6 AcCl + 3 SO2 + 6 HCl + 2 I2 + 4 KCl
or if I2 will be reduced
KICl4 + S + 2 AcOH >> 2 AcCl + SO2 + 2 HCl + KI
[Edited on 10-10-2020 by clearly_not_atara]
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draculic acid69
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| Quote: Originally posted by draculic acid69 | | Quote: Originally posted by Magpie | RCOOH + SOCl2 → RCOCl + SO2 + HCl
SOCl2, thionyl chloride, can be made at home, with much labor. See my "preparation of thionyl chloride," this forum. But SOCl2 is a "3B chemical
weapons" precursor. But, then again, so is PCl3. http://www.australiagroup.net/en/precursors.html
I don't think there is a cheap and easy way to make acid chlorides if that is what you are asking. If it was many here would be doing same. It is
easier to make phosphorus.
[Edited on 21-2-2018 by Magpie] |
In the AA sticky there's info on using sicl4 +GAA---> AA
This is easier to make than socl2+legal+ not sure to buy |
That should be not sus to buy.damm spellcheck.
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draculic acid69
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| Quote: Originally posted by Chemi Pharma | | Quote: Originally posted by FireLion3 | | You said you were in Latin America? Are the regulations strict there? In the US there's not that many chemicals that require filling out a bunch of
paperwork to get, unless someone is trying to purchase known precursor chemicals, or purchasing ridiculous quantities of watched chemicals. For the
most part the US chemical market is pretty open. At least in my opinion. I know other countries out there are far more regulated, especially in
Europe. |
Here in Brazil we have three kind of regulations: The first one is dicted by Army Forces and control the chemical weapons precursors. Private persons
can by only 02 kgs at maximum, filling papers and attaching their documents, explaining why they have a legitimate use to that chemical.
The second one is dicted by Federal Police Department (our FBI) and control the maximum quantities of chemicals that are common employed as precursors
of narcotics manufactory. Private persons can purchase monthly a few quantities without a special licence required.
The third one is dicted by the public health autorities (here called ANVISA), and restrict the commerce and manufacturing of legal psichoative
chemical compounds. License is always required. The bureau also maintain a monthly list containing the banned drugs, alkaloids and narcotics for
criminal law enforcement use.
The most of chemical reagents is free to purchase without restrictions and you can do that easily at chemical supliers or even on the NET. I know that
many other countries like Australia get almost anything under strict control. southern Asia too. East european countries as far as I know have the
most liberal rules worldwide.
May be would be interesting to create a thread about the chemical restrictions existing nowadays in every country, just for fun.
[Edited on 25-2-2018 by Chemi Pharma] |
I seen acetyl chloride pop up on a list of chems available to average Joe
otc from a well known Chem supply here in oz. I thought it was on the
No-go list like acetic anhydride but there it was at a greatly increased price
of course.$700 a litre.
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clearly_not_atara
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| Quote: | In the AA sticky there's info on using sicl4 +GAA---> AA
This is easier to make than socl2+legal+ not sure to buy |
SCl4 is stable only below -30 C. It is produced by adding liquid chlorine to sulfur with strong cooling. Arguably this is easier than SOCl2 via oleum
etc but it is very equipment-intensive in that it requries condensing Cl2 and working with it.
The methods where chlorine gas is introduced to a suspension of S in GAA do not make SCl4, but they do effectively transfer four electrons from one
sulfur atom to four chlorine atoms. I imagine they also have the potential to produce significant amounts of chloroacetic acid and its chloride.
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draculic acid69
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| Quote: Originally posted by clearly_not_atara | | Quote: | In the AA sticky there's info on using sicl4 +GAA---> AA
This is easier to make than socl2+legal+ not sure to buy |
SCl4 is stable only below -30 C. It is produced by adding liquid chlorine to sulfur with strong cooling. Arguably this is easier than SOCl2 via oleum
etc but it is very equipment-intensive in that it requries condensing Cl2 and working with it.
The methods where chlorine gas is introduced to a suspension of S in GAA do not make SCl4, but they do effectively transfer four electrons from one
sulfur atom to four chlorine atoms. I imagine they also have the potential to produce significant amounts of chloroacetic acid and its chloride.
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I know I should be using capital letters and being more accurate for this exact reason:
It's silicon tetrachloride I wrote as sicl4 in the above paragraph.scl4 is close. sicl4 is not sus to buy.
It's seems the easiest way to acid chlorides in my opinion without using hard to obtain,
rare,smelly,toxic or restricted chems.It could also be made in an amatuer setting.sulfur chlorides "can" also be made in amatuer settings but if U
live with or near other ppl or U care at all about the habitability of the structure U r using for chemistry U probably shouldn't make sulfur
chlorides in an amatuer setting.
[Edited on 20-10-2020 by draculic acid69]
[Edited on 20-10-2020 by draculic acid69]
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draculic acid69
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Anyway for theoretical interest in trying to make acid chlorides with out to much toxic smelly middle stages above it says one molecule of sulfur to
two molecules of gaa,
Now how much sulfur is this in grams as sulfur like phosphorus which is P4 or bromine which is usually br2 sulfur is usually represented as S8 or
something so how many grams sulfur would one use for this? I'm a bit confused when it comes to this.
Is it 32grams or 8times this?
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njl
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That's a really interesting question that I'd also like to have answered. That said, as long as the different allotropes of sulfur react in the same
way in this situation, it shouldn't matter. Don't worry about how many sulfur atoms are in a molecule, as long as you are using the molar mass of a
single sulfur atom your math will work out.
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clearly_not_atara
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It's wrong when it says one molecule of sulfur, basically. It should say one mole of sulfur atoms. You need to reduce one mole of chlorine to
eliminate one mole of water; formally:
Cl2 + H2O + 2 e- >> 2 HCl + O(2-)
Each sulfur atom provides four electrons:
S + 2 O(2-) >> SO2 + 4 e-
Neither reaction is actually possible without the other but they do happen in tandem. Naturally you get one mole of anhydride for consuming one mole
of water.
So you get two moles of Ac2O per gram-atom of S alternatively 16 moles Ac2O for one mole S8.
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draculic acid69
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So how many grams of yellow garden product does one put in the flask with the 120 grams of acetic acid?
Also clearly not atara I was referring to the above synth of the acid chlorides where sulfur is used in place of phosphorus not the synth of the
anhydrides.it seems that the rxn of sulfur halides with the sodium salts of carboxylic acids goes all the way to anhydride but with just the free acid
it only makes the acid chloride.no sodium to absorb the halide no anhydride.
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njl
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Most garden sulfur is grossly impure as far as I know, including metal impurities that could interfere with your reaction. I don't know of many good
ways to purify sulfur other than recrystallization from hot toluene which is a pain in the ass due to low solubility. That doesn't mean it isn't worth
a try, but just something to keep in mind.
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draculic acid69
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Let's just say that is irrelevant.can anyone clearly state how many grams of sulfur powder go in the flask?
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clearly_not_atara
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One mole of Ac2O or one mole of AcCl makes no difference; you just add or subtract HCl (easy).
But really you want an excess of AcOH. Otherwise your reaction mixture will probably boil away! AcCl has a low boiling point and the rxn between S and
Cl2 is quite exothermic. What I can tell you is that 16 grams of sulfur will produce, theoretically, about 78.5 grams of acetyl chloride from 60 grams
of acetic acid and should probably be used with oh I don't know 120 grams of AcOH might be safe, just keep an eye on the temperature ^,~
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mr_bovinejony
Hazard to Others
Posts: 130
Registered: 20-4-2018
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Mood: ASS
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I've been thinking about this one lately and after seeing chem players video could anhydrous oxalic acid be substituted for gaa? I'm not sure of the
solubility of oxalic acid in acetonitrile but surely there must be a solvent that can dissolve the acid and be miscible with acetonitrile
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