What concentration hbr in acetic did you get? I can get 33%
Re: Jon's route
« Reply #140 on: March 22, 2013, 10:27:54 AM »
Topic: Jon's route (Read 3445 times)
myhero
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Electro´S
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Re: Jon's route
« Reply #141 on: March 22, 2013, 10:50:24 AM »
Ok, with Pure reagents it´s looks like "shake´n bake".
But had any bee, done the workup properly?
for example, filtering HBr/Acetic acid from the sodium salts, is a good point to start. And drying the methyl amine/IPA solution prior to use would be the best before the end.
I´m not sure, but I have not read a single reference from a new bee using dried IPA/methylamine in the proper concentration, so all the fails are just Fails, and just probe inexperience hands.
All the workup is simple and cheap. Just spend your time and money in the methyl amine solution.
But had any bee, done the workup properly?
for example, filtering HBr/Acetic acid from the sodium salts, is a good point to start. And drying the methyl amine/IPA solution prior to use would be the best before the end.
I´m not sure, but I have not read a single reference from a new bee using dried IPA/methylamine in the proper concentration, so all the fails are just Fails, and just probe inexperience hands.
All the workup is simple and cheap. Just spend your time and money in the methyl amine solution.
T-cowboy
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Re: Jon's route
« Reply #142 on: March 22, 2013, 10:55:25 AM »
yes electro is straight right on this one, drying amines can complex them if you do it with a salt.
Suggestion: just search for methylamine solution in any alcohol. Jon mentions IPA only works, but no no. he says steric hindrance and what so ever.
but heres a trick for you ALL on this route.
get yourself some triethylamine and menh2.hcl. mix it in IPA/ETOH, this will freebase the men2h into the solution without making water. pkb is stronger. you could filter this triethylamine.hcl of, but it isnt that nucleophilip.
Suggestion: just search for methylamine solution in any alcohol. Jon mentions IPA only works, but no no. he says steric hindrance and what so ever.
but heres a trick for you ALL on this route.
get yourself some triethylamine and menh2.hcl. mix it in IPA/ETOH, this will freebase the men2h into the solution without making water. pkb is stronger. you could filter this triethylamine.hcl of, but it isnt that nucleophilip.
T-cowboy
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Re: Jon's route
« Reply #143 on: March 22, 2013, 10:56:07 AM »
33 % acetic hbr is the norm. and it really works mehyro.
T-cowboy
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Re: Jon's route
« Reply #144 on: March 22, 2013, 11:28:22 AM »
Weird thing though, i know bromosafrole is bichromatic in different puritys. but i have noticed that off all the pics here on the site. bromosafrole is brown dark. with high purity (vac distil, powerfull vac.) the color is transparent, and slightly orange. maybe thats the issue. ( crap in, crap out )
EMTWC
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Re: Jon's route
« Reply #145 on: March 23, 2013, 11:05:46 AM »
tar indicates sitting too long, but it didn't go more than 23-24 hours...going to keep at it
T-cowboy
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Re: Jon's route
« Reply #146 on: March 24, 2013, 01:30:01 AM »
Okay this will be my last post regarding jons route, ( maybe t-cowboy is the new jon? becasue it seems i have been able to pull whis of.)
Get your safrole oil, from any source. BUT please ocotea cymabrum-
Get yourself hold of 33 % hrb acetic acid. dont hassle with the stoich. its easy to get hold of,
Then you know the drill. Also described in TS2 by strike.
Flood with water, separate and then dry it with a haridryér or hotair oven set on LOWEST temp.
Now, here are two options:
MEnh2 .hcl put this in IPA or ABOSLUTE ethanol, now ad triethylamine. this will liberate menh2 gas without generating water. Hence annydrous
One can get your hands on 33% menh2 in absolute ethanol,
The iodosafrole can be a hassle, and please avoid it. just use the bromo. its a good leaving group. I-->Br---> and so forth. because distilling/evap acetone is a bitch. and then separate and dry.. (no water remember whatsoever)
Now one just does what is the easiest. mix it up baby. let it sit for 5-6 days, if your not planing pressure vessels and heat. BOOOM
Now this is new:
After it has reacted bromide salt WILL be in solution. so filter (vac)
Now remember we now have the mdxx in the solution, drip muriatic acid until ph6. if you cannot see precipitation, then just evap, or just A/B.
Thats it.
GIVE HONEY i really like honey, in real life too!!
Get your safrole oil, from any source. BUT please ocotea cymabrum-
Get yourself hold of 33 % hrb acetic acid. dont hassle with the stoich. its easy to get hold of,
Then you know the drill. Also described in TS2 by strike.
Flood with water, separate and then dry it with a haridryér or hotair oven set on LOWEST temp.
Now, here are two options:
MEnh2 .hcl put this in IPA or ABOSLUTE ethanol, now ad triethylamine. this will liberate menh2 gas without generating water. Hence annydrous
One can get your hands on 33% menh2 in absolute ethanol,
The iodosafrole can be a hassle, and please avoid it. just use the bromo. its a good leaving group. I-->Br---> and so forth. because distilling/evap acetone is a bitch. and then separate and dry.. (no water remember whatsoever)
Now one just does what is the easiest. mix it up baby. let it sit for 5-6 days, if your not planing pressure vessels and heat. BOOOM
Now this is new:
After it has reacted bromide salt WILL be in solution. so filter (vac)
Now remember we now have the mdxx in the solution, drip muriatic acid until ph6. if you cannot see precipitation, then just evap, or just A/B.
Thats it.
GIVE HONEY i really like honey, in real life too!!
BeeGirl
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Re: Jon's route
« Reply #147 on: March 25, 2013, 02:57:48 PM »
15 gallons of GAA goes for $199 ($11 for 950 ml)
An oz of hydrobromic acid is $16.50.
the savings is worth the stoich hassles, especially for those working out the route.
what are you using for a pressure vessel, wally world extinguisher? Or something improvised or more permanent.
When the wasps start hitting the 92% yields maybe they can start ponying up for hydrobromic acid
give you honey just for keeping hope alive
An oz of hydrobromic acid is $16.50.
the savings is worth the stoich hassles, especially for those working out the route.
what are you using for a pressure vessel, wally world extinguisher? Or something improvised or more permanent.
When the wasps start hitting the 92% yields maybe they can start ponying up for hydrobromic acid
give you honey just for keeping hope alive
zgoat65
- Subordinate Wasp
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Re: Jon's route
« Reply #148 on: March 26, 2013, 12:45:36 AM »
I've done a lotta readin on this route, and havin discussions with folks who have done it. Word on the street is, there's a wasp that does "jon's route" (and gets the 90% yield) in 5gal buckets. So festerz fire extinguisher what-not would work too if one had enough oil to experiment with. The 5gal bucket thing may just bee forum lore, but i doubt it. I tend to believe the dude that said it.
BeeGirl
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Re: Jon's route
« Reply #149 on: March 26, 2013, 12:35:41 PM »
festers method was debunked by jon (and the eleusis pie fight), but jon still talks about getting 2 or 3 uses out of a fire extinguisher.
5 gallon bucket seems potentially appropriate...thanks
5 gallon bucket seems potentially appropriate...thanks
RhinoJackson
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Re: Jon's route
« Reply #150 on: March 27, 2013, 02:04:51 AM »
I've done a lotta readin on this route, and havin discussions with folks who have done it. Word on the street is, there's a wasp that does "jon's route" (and gets the 90% yield) in 5gal buckets. So festerz fire extinguisher what-not would work too if one had enough oil to experiment with. The 5gal bucket thing may just bee forum lore, but i doubt it. I tend to believe the dude that said it.
What about drdeepwood/ron paul? He'll sell you his notes for this method, only $500 in bitcoins!
BeeGirl
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Re: Jon's route
« Reply #151 on: March 27, 2013, 02:17:29 AM »
people will sell anything for bitcoins, especially these dayz.
can you confirm the info reliable? why not post it and diminish its value asap?
one has to suspect its a conglomerate of the info already available to the savy searcher.
but hey, Rhino, we're all ears (or eyes she supposes). do tell...
can you confirm the info reliable? why not post it and diminish its value asap?
one has to suspect its a conglomerate of the info already available to the savy searcher.
but hey, Rhino, we're all ears (or eyes she supposes). do tell...
RhinoJackson
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Re: Jon's route
« Reply #152 on: March 27, 2013, 02:34:09 AM »
people will sell anything for bitcoins, especially these dayz.
can you confirm the info reliable? why not post it and diminish its value asap?
one has to suspect its a conglomerate of the info already available to the savy searcher.
but hey, Rhino, we're all ears (or eyes she supposes). do tell...
I don't think it's anything we don't know. It's just his write-up (a la doctordrool/brightstar) of Jon's route. I think most failures are due to poor procedure. Anhydrous conditions and slight pressure on the amination seem to be key.
BeeGirl
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Re: Jon's route
« Reply #153 on: March 27, 2013, 02:50:21 AM »
a good thorough write up is needed...all threads go dry it seems...even this one; the beginning stoichiometry is never revealed...what are IGT's numbers? Fractal?
look at other threads and things are rather inconsistent:
btjuice in his thread here
50g Safrole
57.4g H2SO4
66.6g NaBr
71.1g Glacial Acetic Acid
IWGT in re-visit pnaut thread
20g safrole
98g H2SO4
103g NaBr
405 GAA
salat in Yeee Haaah
15 ml brazillian sassafras oil (not cleaned up)
35 ml Sulfuric acid
75 g NaBr
100 ml GAA
***eventually added 80 ml more GAA to get enough to stir, 20 more g NaBr, and 10 ml more sulfuric acid.
15
45
95
180
there is some ml to gm conversion on the last one, but each of them have different stoich.
look at other threads and things are rather inconsistent:
btjuice in his thread here
50g Safrole
57.4g H2SO4
66.6g NaBr
71.1g Glacial Acetic Acid
IWGT in re-visit pnaut thread
20g safrole
98g H2SO4
103g NaBr
405 GAA
salat in Yeee Haaah
15 ml brazillian sassafras oil (not cleaned up)
35 ml Sulfuric acid
75 g NaBr
100 ml GAA
***eventually added 80 ml more GAA to get enough to stir, 20 more g NaBr, and 10 ml more sulfuric acid.
15
45
95
180
there is some ml to gm conversion on the last one, but each of them have different stoich.
RhinoJackson
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- Posts: 4
Re: Jon's route
« Reply #154 on: March 27, 2013, 02:58:54 AM »
a good thorough write up is needed...I think many would disagree. All we need is one more mdma synth for dummies...
BeeGirl
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Re: Jon's route
« Reply #155 on: March 27, 2013, 03:08:40 AM »
any comment on the stoich?
Whale
- I can ride my bike with no handlebars
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Re: Jon's route
« Reply #156 on: March 27, 2013, 04:29:33 AM »
Regarding the stio:
According to jons original post
1mol safrole:1.9mols HBr in 40% GAA soln
162g safrole:153.4g HBr in 383.5g of GAA
now to get that 153.4g of HBr we're gunna need NaBr nd H2SO4
NaBr (s) + H2SO4 (aq) ? HBr (aq) + NaHSO4 (aq)
2 HBr (aq) + H2SO4 (aq) ? Br2 (g) + SO2 (g) + 2 H2O (l)
Soooo we dont want excess sulfuric. its 1mol:1mol so mebbe add a bit more NaBr (1.1mols?) to make sure theres no bromine made
113g NaBr:98g H2SO4
According to jons original post
1mol safrole:1.9mols HBr in 40% GAA soln
162g safrole:153.4g HBr in 383.5g of GAA
now to get that 153.4g of HBr we're gunna need NaBr nd H2SO4
NaBr (s) + H2SO4 (aq) ? HBr (aq) + NaHSO4 (aq)
2 HBr (aq) + H2SO4 (aq) ? Br2 (g) + SO2 (g) + 2 H2O (l)
Soooo we dont want excess sulfuric. its 1mol:1mol so mebbe add a bit more NaBr (1.1mols?) to make sure theres no bromine made
113g NaBr:98g H2SO4
BeeGirl
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Re: Jon's route
« Reply #157 on: March 27, 2013, 10:53:16 PM »
those numbers lean towards IWGT in the infamous re-visit thread EXCEPT for one minor detail
IWGT = 20g safrole
jon = 162g safrole
are we accounting for 93% H2SO4, which is the OTC avail?
IWGT = 20g safrole
jon = 162g safrole
are we accounting for 93% H2SO4, which is the OTC avail?
Whale
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Re: Jon's route
« Reply #158 on: March 27, 2013, 11:34:12 PM »
i was accounting for 98% sulfuric
BeeGirl
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Re: Jon's route
« Reply #159 on: March 28, 2013, 12:43:06 AM »
most OTC test out higher, but claims 93%