10-29-03 17:39
No 467712
Could Sodiumdichromate replaced with potassiumdichromate
without any consequences in that Codeine to
14-Hydroxycodeinone synth?
../rhodium /oxycodo
Then swim would like to know if Dibrommethan could make
the same job instead of methansulfonic acid (Tribrommethan)in the further Oxymorphone synth?
Swim was very happy if some bee out there could answer
this question.
Maybe dope_amine hisself made experience in that case,
but any other suggestion will be welcome of course.
(Hive Addict)
10-29-03 22:55
No 467758
sounds like some toxic shit.
I'm not aware of a substitue for methane sulfonic acid, exept another alkyl or aryl sulfonic acid like tosic acid for example.
Methylsulfonylmethane MSM ( the methyl ester of methane sulfonic acid) could possibly be coverted into methane sulfonic acid by hydroylisis.
with a base for instance then you could liberate the methane sulfonic with a stronger acid.
(Stranger)
10-31-03 03:57
No 467985
thanks a lot SPISSHACK.
The infos about that Tribrommethan is absolutly wrong
in my post.
I had made a quick search with the metanesulfonic acids CAS NO (75-75-2) and found out now that some idiots
have mixed up it with 75-25-2 that is the CAS of Tribrommethan.
(Soothsayer)
10-31-03 15:50
No 468040
Synonyms: amidosulfonic acid, amidosulfuric acid, sulfamidic acid, sulphamic acid
Molecular formula: H3NO3S
CAS No: 5329-14-6
EC No: 226-218-8
This is sold at my local hardware store in purity, If only hey,.
Every time I make love to my sister, I feel that this truly is a drug within itself
(Stranger)
11-02-03 15:24
No 468396
Thanks for info hellman
But swim is happy with that tosic acid.
(p- Tolylsulfonic acid) CAS 104-15-4
(Stranger)
11-24-03 06:36
No 472867
Lone Ranger's hydroxycodeinone synth calls for sodium dichromate. SWIM knows someone that has plenty of LG ammonium dichromate. (NH4)2Cr2O7 has a water solubility of 40g/100g, while Na2Cr2O7.2H2O has a water solubility of 185g/100g. Could more ammonium dichromate be used (haven't done the math yet) to compensate for this lesser solubility? If so, would there be any other problems in swim's friend using ammonium dichromate to form chromic acid for this synth?
Am a chemhack, so if a flame is in order, please ignite torches now!
Otherwise, would like to thank The Hive immensely for providing such an incredible site.
(Stranger)
12-01-03 18:11
No 474197
Only the dichromate does the oxididation,
so ammoniumdichromate should do the same work.
But don`t ask me about the amount..
But in further reference with the Patent DE411530
I found out, that Lone Ranger had exactly copied
this german patent.
His writeup also uses the same amounts except
for the codein, which is stated with 20g (parts)in the original not 30.
Is this a big spelling error?
By the way. Why do you not use dope_amins version?
But it uses Lone Rangers amounts as well.....
except without the chromic acid step.
So the amount problem doesn`t change.
(Stranger)
12-03-03 07:21
No 474495
thank you BM for your reply. SWIM will attempt synth with (NH4)2Cr2O7 and see what happens.
When you refer to Dope Amine's synth, do you mean the one that was (I think) oringinally posted on poppies.org? It starts with "Hey you fuckheads..."?
D_A doesn't state any amounts/ratios in this write-up, only temperatures & times. Think SWIM will probably decide to try the Lone Ranger's synth verbatim. It could be a typo, but the Ranger seems to know what he's talking about.
(Stranger)
12-04-03 09:26
No 474665
Well dope_amins version refers to Lone Rangers amounts.
And yes: itīs that one from poppies..(Hey you fuckheads...)
Didn`read it at rhodium`s site?
It says:
" Codeine --> Oxycodone
by dope_amine
Codeine -> 14-Hydroxycodeinone
Dissolve your codeine base in the acid solution (acetic, we're following the method given in Lone Ranger's procedure above, so use those amounts) in a rb flask and set it in an ice water bath with stirring. Now that it's nice and cool, slowly pipette in the dichromate solution. The solution immediately turns a milky orange/yellow.
Now......."
But as I think he scaled Lone Rangers amounts down to
make this synth with less codein.
ref. Dope_Amine : "I have done this on a few gram scale so there wasn't a lot of hydrogen absorbed. If you were doing a tens of grams scale, you would need to refill the balloons several times during the reaction or you may still need to do this if you have bad leaks"
So this also indicates that it works fine with just 3grams
codein.
For the NaCr2O7 substution matter, I found this at poppies:
Pheesees asked: -"Sodium dichromate has a water solubility of 4.9G/100ml. How does one get 20G into 25ml?"
Guru answered:-"Even though a compound has a certain solubility, someone can still make a saturated or supersaturated solution with it. It takes 111.4gr of Na2Cr2O7/100ml @ 18° to make a saturated solution so the chemist shouldn't have a problem dissolving 20gr of Na2Cr2O7 in 25ml and if they do then they can heat it up a little bit to help it dissolve...."
Pheesees replied: - "That info helps a lot! I was going to substitute KCr2O4 for the sodium salt, but didn't realise the differences in solubility...my info didn't include solubility for the sodium salt."
Unfortunately I donīt have the url of this conversion,
because I just copied it.
(Stranger)
12-05-03 07:13
No 474820
thanks for that info BM. The more swim thinks about it, the more he thinks that the solubility of the dichromate salt is probably pretty important.
Just read a post by Elementary (post no. 258966). It describes converting ammonium dichromate to potassium or sodium dichromate. Didn't realise it was this simple. Thank you Elementary.
BM, Dope Amine talks about performing Ranger's synth on a smaller scale (ie a few grams of codeine). Swim thinks this would be OK if one had enough experience (swim doesn't). From swim's meth adventures, nanos' can get nasty.
(Stranger)
12-05-03 08:34
No 474832
There isn`t much info out here in the Hive about
this unpopular synth.
It seems that we are the only two at this time.....
There is also a thread in the Methods Dicourse,
which of course uses other synth routes and chemicals. Maybe you take a look at it.
However by searching the Hive I found Bulldog44`s 2 years old posts.
Post 256825 (Bulldog44: "Need help.", Methods Discourse)
Post 267113 (Bulldog44: "Re: So what the hell is it ??", Methods Discourse)
He did a nano with about 0.5 g starting codi.
Two month later he said he didnīt have lot success.
Post 300426 (Bulldog44: "update", Methods Discourse)
I will give it a try with about 3g.
You said the solubility is pretty important.
What do you think how much water is necassary
for 2g K2Cr2O7?
Since the Potdichrom. has a very less solubility
than NAdichrom. About 5g/100ml H2O.
I would try it with 2g and 50ml water.
Or what do you think? Would the increasing of water amount
harm the synth in any way
(Stranger)
12-08-03 15:19
No 475511
yeah, this synth does seem to be fairly unpopular.
Swim don't have enough experience to advise you.
Waiting on some GAA, then it might be time to get hands dirty.
BM, are you from oz?
(Stranger)
12-09-03 05:27
No 475626
swim did a first trial with about 1,5 g starting codi.
1,2g KaCr2O7 did not dissolve well in 10ml water
so he took in another 10ml and shaked a bit then.
It then dissolved all well.
swim was a little confused about that german patent
which was stated with 20g Codi and 20g Dichromate.
So he thought it was the best to use the middle.
After all he got a dark brown liquid that is forming
now crystels from time to time.
The extarction with CH2Cl2 first formed an emulsion.
Donīt shake to hard in that way.
But you can break the emulsion with another load of
solvent or just waiting and slowly pipette out the
clearly yellow solvent(brown when dissolved in a small amount of solvent).
Iīm waiting now for my Pd/C to go ahead with the
hydrogeneration.
oz is Australia, right?
swim comes from a european country where all good chemists
came from and now
with me they come from
.