Swisneak wil pray for your success 
Re: Dr Drool method Viable?
« Reply #100 on: March 28, 2013, 05:50:28 PM »
Topic: Dr Drool method Viable? (Read 2303 times)
Sneak
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ImAMANGUYS
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Re: Dr Drool method Viable?
« Reply #101 on: March 28, 2013, 05:56:09 PM »
All your questions so far answered and more:
http://127.0.0.1/talk/index.php/topic,2699.0.html
Read up man, itll help you tons.
http://127.0.0.1/talk/index.php/topic,2699.0.html
Read up man, itll help you tons.
myhero
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Re: Dr Drool method Viable?
« Reply #102 on: March 30, 2013, 07:57:14 AM »
Questions were answered. All but one. Is it better to use 5% NaOH or 5-10% NaHCO3... ? In the hive I have read about people doing only water washes and getting very high yields...
pbinteger
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Re: Dr Drool method Viable?
« Reply #103 on: April 15, 2013, 12:05:39 AM »
Hi Myhero!
Did you ever have success?
Yields?
_Pbint_
Did you ever have success?
Yields?
_Pbint_
myhero
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Re: Dr Drool method Viable?
« Reply #104 on: April 15, 2013, 08:16:15 AM »
Still need to finish. I will report when done. For sure it's a success. I ll just post yield.
myhero
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Re: Dr Drool method Viable?
« Reply #105 on: April 19, 2013, 09:10:28 AM »
So finally some update.
I washed the post hydrolization fluids with water then with Sodium Bicarbonate 10% then brine. back-extracted all washings with a little DCM and I distilled the DCM out under weak vacuum. Then I moved to higher vacuum for ketone fractional distillation with vigreux column.
At 75°C some oil started to come over. I was not sure what it could be (isosafrole fore-run or ketone) as it looked almost transparent so I kept distilling. Last time I had fore-run but it was because I used weak H2O2. This time proper H2O2 was used so I didn't expect any substantial fore-run. but there could have been a couple of ml and I ll never know.
In the end I collected 253g of pale yellow oil with a slight green hue between 75°C and 84°C (starting from 300g isosafrole) I also dropped by mistake about 10-15ml in the process otherwise actual yield would even be higher, shit!!!). Also last time, the ketone I collected under such strong vacuum was just pale yellow and not too intense in color. I believe it has something to do with the temperature. In the end of the distillation it was becoming more yellow as I was increasing bath temp to try and squeeze all possible ketone out of the distillation flask.
After dismantling the apparatus I poured some peanut oil in the warm distillation flask to prevent the residue from solidifying. It worked. Next time I ll also try to pour it on the inner walls of the flask, not just the bottom, before the water rinse as water immediately forces the residue to become solid and stick to the bloody flask. I am positive there is more ketone in the residue but it's increasingly difficult to squeeze it out. Maybe dissolving the residue in some organic solvent and try to form the bisulfite adduct could push yields up a bit too.
I will do a sodium bisulfite test soon to check the quality of my distillate but to be honest I don't see what else it can be. The temp range is too narrow for it to be 2 different compounds. There was no point in which the distillation stopped and temperature increased. Everything was gradual. all the reactions before this distillation pointed in the right direction in terms of color change and all.
I ll keep you guys posted but so far it looks like very good yields 84% w/w (76%molar yield).
I washed the post hydrolization fluids with water then with Sodium Bicarbonate 10% then brine. back-extracted all washings with a little DCM and I distilled the DCM out under weak vacuum. Then I moved to higher vacuum for ketone fractional distillation with vigreux column.
At 75°C some oil started to come over. I was not sure what it could be (isosafrole fore-run or ketone) as it looked almost transparent so I kept distilling. Last time I had fore-run but it was because I used weak H2O2. This time proper H2O2 was used so I didn't expect any substantial fore-run. but there could have been a couple of ml and I ll never know.
In the end I collected 253g of pale yellow oil with a slight green hue between 75°C and 84°C (starting from 300g isosafrole) I also dropped by mistake about 10-15ml in the process otherwise actual yield would even be higher, shit!!!). Also last time, the ketone I collected under such strong vacuum was just pale yellow and not too intense in color. I believe it has something to do with the temperature. In the end of the distillation it was becoming more yellow as I was increasing bath temp to try and squeeze all possible ketone out of the distillation flask.
After dismantling the apparatus I poured some peanut oil in the warm distillation flask to prevent the residue from solidifying. It worked. Next time I ll also try to pour it on the inner walls of the flask, not just the bottom, before the water rinse as water immediately forces the residue to become solid and stick to the bloody flask. I am positive there is more ketone in the residue but it's increasingly difficult to squeeze it out. Maybe dissolving the residue in some organic solvent and try to form the bisulfite adduct could push yields up a bit too.
I will do a sodium bisulfite test soon to check the quality of my distillate but to be honest I don't see what else it can be. The temp range is too narrow for it to be 2 different compounds. There was no point in which the distillation stopped and temperature increased. Everything was gradual. all the reactions before this distillation pointed in the right direction in terms of color change and all.
I ll keep you guys posted but so far it looks like very good yields 84% w/w (76%molar yield).
some55one
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Re: Dr Drool method Viable?
« Reply #106 on: April 23, 2013, 07:44:14 AM »
Hello Everyone a new bee I have been lurking ever since I found Bright Star's method over a year ago.
Some deeper searching led me to Dr. Drool's Method and only recently have I come across some of the other methods. The only issue is that I have managed to put together pieces of the puzzle that work best for the MM and Dr. Drool's methods.
My method of approaching the MDMA syn are using Dr. Drools method except instead of using the benzo wacker I am going to try Rhodium's K.R.V. which was described by the OP. I do have the components to make p-benzo but I would have to syn from hydroquinone which I am hesitant to do at the moment.
Two items difficult to obtain
1) HgCl2 was pretty difficult would using Hg2Cl2 in the Hg/AL amination suffice?
2) a large separatory funnel, stuck a 250ml, is it possible to decant?
Some deeper searching led me to Dr. Drool's Method and only recently have I come across some of the other methods. The only issue is that I have managed to put together pieces of the puzzle that work best for the MM and Dr. Drool's methods.
My method of approaching the MDMA syn are using Dr. Drools method except instead of using the benzo wacker I am going to try Rhodium's K.R.V. which was described by the OP. I do have the components to make p-benzo but I would have to syn from hydroquinone which I am hesitant to do at the moment.
Two items difficult to obtain
1) HgCl2 was pretty difficult would using Hg2Cl2 in the Hg/AL amination suffice?
2) a large separatory funnel, stuck a 250ml, is it possible to decant?
myhero
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- Posts: 80
Re: Dr Drool method Viable?
« Reply #107 on: April 23, 2013, 08:40:53 AM »
The bisulfite test came out ok. I tested one ml in a test tube with sat.ed. sodium metabisulfite. I am not 100% sure there is no isosafrole in there. I might do a small reductive amination and see the results
carbonated
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Re: Dr Drool method Viable?
« Reply #108 on: April 23, 2013, 02:06:18 PM »
Two items difficult to obtain
1) HgCl2 was pretty difficult would using Hg2Cl2 in the Hg/AL amination suffice?
2) a large separatory funnel, stuck a 250ml, is it possible to decant?
Neither of these items is difficult to obtain for anyone who's spent more than 5 minutes looking for them...
some55one
- Larvae
- Posts: 3
Re: Dr Drool method Viable?
« Reply #109 on: April 23, 2013, 03:09:31 PM »
Two items difficult to obtain
1) HgCl2 was pretty difficult would using Hg2Cl2 in the Hg/AL amination suffice?
2) a large separatory funnel, stuck a 250ml, is it possible to decant?
Neither of these items is difficult to obtain for anyone who's spent more than 5 minutes looking for them...
HgCl2 I couldn't find
The separatory funnel is not hard to find just I did buy a 2000ml just to have it break on me during shipping, still awaiting replacement and my private time to work on my little side project is here and I am without a 2000ml funnel
fractal
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Re: Dr Drool method Viable?
« Reply #110 on: April 23, 2013, 04:58:55 PM »
You can use other salts of mercury, they have lower solubility but still work fine.
zgoat65
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Re: Dr Drool method Viable?
« Reply #111 on: May 02, 2013, 01:57:32 AM »
Afoaf makes his own Hg salts for reductive amination. As long as one has a fume hood (ghetto or bought) that is working, then working with Cl2 gas shouldn't bee a problem, and there is a good synth for Hg2Cl2 on rhodium.
OR an old bee told me about this little trick:
an easy way to amalgamate aluminium:
Get some DCDBDMH. Get a test tube and place a couple of pinhead sized drops of Hg into it. Crack off a chunk of the Spa bromiator and place in test tube. Plug tube with some glass wool. Heat tube with a flame until evolution of BrCl and bromine is observed.Tilt test tube diagonal so Hg droplet is exposed to pool. When bromine ceases to evolve, let the whole thing cool and solidify. Fill tube half way with EtOH and agitate solidified mass as much as possible with a skewer through glass wool. With gloved finger shake that tube for a while. Let settle. Carefully decant Hg laden EtOH onto Pre-cleaned Aluminium. Obsevre dulling of Aluminium. Remove from Toxic EtOH/Hg mix and rinse in clean EtOH. Use for what ever purpose.
OR an old bee told me about this little trick:
an easy way to amalgamate aluminium:
Get some DCDBDMH. Get a test tube and place a couple of pinhead sized drops of Hg into it. Crack off a chunk of the Spa bromiator and place in test tube. Plug tube with some glass wool. Heat tube with a flame until evolution of BrCl and bromine is observed.Tilt test tube diagonal so Hg droplet is exposed to pool. When bromine ceases to evolve, let the whole thing cool and solidify. Fill tube half way with EtOH and agitate solidified mass as much as possible with a skewer through glass wool. With gloved finger shake that tube for a while. Let settle. Carefully decant Hg laden EtOH onto Pre-cleaned Aluminium. Obsevre dulling of Aluminium. Remove from Toxic EtOH/Hg mix and rinse in clean EtOH. Use for what ever purpose.
carbonated
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Re: Dr Drool method Viable?
« Reply #112 on: May 14, 2013, 05:36:54 AM »
I should be attempting this route soon but I'm a little worried my 35% H2O2 figure is actually in a smaller concentration than advertised. Would it be better to overcompensate my numbers or just hope for the best?
Flight
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Re: Dr Drool method Viable?
« Reply #113 on: May 21, 2013, 04:43:19 AM »
I just started the isomerization and will be following this procedure the rest of the way, http://parazite.nn.fi/hiveboard/newbee/000528375.html
Isomerization went as follows:
~5g of pestled 90% KOH was added to ~190ml of Oil. Temperature was brought up to 190 for 2 hours then lowered to 140-150 and stirred for 24 hours. Immediately after adding KOH the oil turned color (kinda brownish). After 24 hours vacuum was connected and distillation began. Everything came over at about 118 (recirculating aspirator used for vacuum). Ran out of ice and stopped distillation. BP of distillate was ~245. The next day KOH was filtered off and the remaining oil was distilled. Remainder all came through the condenser at about 120-124. Isomerization was a success. Not sure of the total amount yet, will check tomorrow, but yield should be pretty good.
Original distillate was tested at atmospheric pressure to get a good idea of BP, (245+). Oil turned from clear to a light yellow at the high temp. Hopefully this won't be a problem for future steps, not sure if the colors will match Ocotea's pictures exactly since the Iso isn't clear anymore.
Isomerization went as follows:
~5g of pestled 90% KOH was added to ~190ml of Oil. Temperature was brought up to 190 for 2 hours then lowered to 140-150 and stirred for 24 hours. Immediately after adding KOH the oil turned color (kinda brownish). After 24 hours vacuum was connected and distillation began. Everything came over at about 118 (recirculating aspirator used for vacuum). Ran out of ice and stopped distillation. BP of distillate was ~245. The next day KOH was filtered off and the remaining oil was distilled. Remainder all came through the condenser at about 120-124. Isomerization was a success. Not sure of the total amount yet, will check tomorrow, but yield should be pretty good.
Original distillate was tested at atmospheric pressure to get a good idea of BP, (245+). Oil turned from clear to a light yellow at the high temp. Hopefully this won't be a problem for future steps, not sure if the colors will match Ocotea's pictures exactly since the Iso isn't clear anymore.
myhero
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Re: Dr Drool method Viable?
« Reply #114 on: May 21, 2013, 08:04:00 AM »
you ll be ok flight. That perfect.
Flight
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Re: Dr Drool method Viable?
« Reply #115 on: May 21, 2013, 06:18:54 PM »
Remaining Iso combined with the first batch and the total is 140.70g. About a 75% conversion, not bad considering it was the first attempt and it was a success. Also, a lot of Iso was probably filtered off with the KOH as a good wash was not performed.
The dilemma now is that the writeup calls for 300g (or half, 150g) Iso to form the glycol for the next step. Is this ~10g going to be a huge issue, or should I wait and convert more Iso?
The dilemma now is that the writeup calls for 300g (or half, 150g) Iso to form the glycol for the next step. Is this ~10g going to be a huge issue, or should I wait and convert more Iso?
AoicVH
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Re: Dr Drool method Viable?
« Reply #116 on: May 21, 2013, 06:29:16 PM »
Just do your synthesis with a factor of 140/150=0,933
So if you synthesis calls for 45ml X you calculate 0,933*45=42 and so on
So if you synthesis calls for 45ml X you calculate 0,933*45=42 and so on
myhero
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Re: Dr Drool method Viable?
« Reply #117 on: May 22, 2013, 01:49:24 PM »
Exactly just scale everything accordingly...
Allyl
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Re: Dr Drool method Viable?
« Reply #118 on: May 25, 2013, 06:41:18 PM »
Hey Flight,
How did you go about testing BP at such high temps? Seems to be too high for a test tube bath, and I doubt you'd want to waste any oil that could possibly degrade at high temps on a micro distillation. Test tube in a sand bath, perhaps?
Or did you just calculate it based on the bp at decreased pressure?
How did you go about testing BP at such high temps? Seems to be too high for a test tube bath, and I doubt you'd want to waste any oil that could possibly degrade at high temps on a micro distillation. Test tube in a sand bath, perhaps?
Or did you just calculate it based on the bp at decreased pressure?
Flight
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Re: Dr Drool method Viable?
« Reply #119 on: May 29, 2013, 05:13:11 PM »
Allyl,
Though it's not recommended (because it isn't all that safe), I have no problem getting an oil bath to 260+ with my hot plate.
Just completed the hydrolysis, the washing and back washing. About 210g of glycol was hydrolized, the organic layer washed with 3x 200ml dH2O, 2x 300ml 5% NaOH, followed by another 200ml dH2O and finally 200ml brine. The aqueous layers pooled and back extracted 2x 100ml DCM, followed by 200ml dH2O and finally 200ml brine.
The back extracted pool is a medium color yellow, so there must be some goodies in there. There was no issue with emulsion when running the basic washes. The original oil/DCM will be combined with the back washed pool of DCM and stripped. Hopefully once stripped vacuum will be connected and yields of ketone will be posted.
For anyone else that has back washed the aqueous layers does that color seem right (medium yellow)? The original organic layer went from black/dark red to a bit of a lighter color after the basic washes.
Thanks,
Flight
Though it's not recommended (because it isn't all that safe), I have no problem getting an oil bath to 260+ with my hot plate.
Just completed the hydrolysis, the washing and back washing. About 210g of glycol was hydrolized, the organic layer washed with 3x 200ml dH2O, 2x 300ml 5% NaOH, followed by another 200ml dH2O and finally 200ml brine. The aqueous layers pooled and back extracted 2x 100ml DCM, followed by 200ml dH2O and finally 200ml brine.
The back extracted pool is a medium color yellow, so there must be some goodies in there. There was no issue with emulsion when running the basic washes. The original oil/DCM will be combined with the back washed pool of DCM and stripped. Hopefully once stripped vacuum will be connected and yields of ketone will be posted.
For anyone else that has back washed the aqueous layers does that color seem right (medium yellow)? The original organic layer went from black/dark red to a bit of a lighter color after the basic washes.
Thanks,
Flight