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Author Topic: Dr Drool method Viable?  (Read 2303 times)

pbinteger

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Re: Dr Drool method Viable?
« Reply #60 on: January 30, 2013, 04:14:09 PM »
@myhero:

After separating the organic layer from the aqueous directly after hydrolysis, and then extracting the aqueous layer several times with a non-polar solvent, the next step is to wash with 5% NaOH.

I do this NaOH wash twice. After each wash -- giving at least 20 minutes for the oil / DCM to separate -- I then combine the aqueous / NaOH layers and back extract them thrice with ~100mL DCM -- this certainly increases yields.

Then I wash the DCM / Oil with water --> then brine --> and back extract those aqueous layers as well with small amounts of solvent. Then I strip the solvent with the rotovap and set up for fractional distillation. It takes a long time with all the waiting and swirling but it pays off in yields.

_Pbint_

myhero

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Re: Dr Drool method Viable?
« Reply #61 on: January 31, 2013, 09:48:49 AM »
good I ll certainly try that ... Thanks pbinteger.

akcom

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Re: Dr Drool method Viable?
« Reply #62 on: February 07, 2013, 09:22:17 AM »
Quote from: jon on December 31, 2012, 10:42:37 PM
sometimes when you distill ketones leftover bases can cause aldol style condensations especially if you distill it hot.
so make sure your water washes come out neutral and some of your shit can be partially soluble in water so back extract always.
Excess acid can cause this as well.  Leads to a red color in your distillate that darkens slightly over time

Whale

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Re: Dr Drool method Viable?
« Reply #63 on: February 07, 2013, 01:57:49 PM »
Make sure when washing with DCM if there are any emultions forming just add a bit of noniodized salt and let it sit.

ImAMANGUYS

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Re: Dr Drool method Viable?
« Reply #64 on: February 27, 2013, 03:24:00 AM »
Quote from: pbinteger on December 21, 2012, 11:40:25 PM
I just re-ran the boiling point test -- in a test tube -- w/ my new thermometer.

the safrole boiled at 232 on the dot.

the isosafrole boiled at ~240

pretty good indication of what i've got here.

Hm...Is it typical for iso to come over around ~240? I only ask because the file in the rhodium archive states the BP of IsoSaf to be 153 for one of the isomers.

I'm asking because some recently created iso boiled at 243*c at atmospheric pressure. Maybe someone with more experience can speak up. I plan to test the "iso" later tonight with a drip into sulfuric, but wanted to hear other member experience.

Eternal thanks!

The learning Ima.

Whale

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Re: Dr Drool method Viable?
« Reply #65 on: February 27, 2013, 03:34:35 AM »
Iso should be boiling around 253C at atmospheric pressure.
Ref:http://www.erowid.org/archive/rhodium/chemistry/isomerizafrole.html

ImAMANGUYS

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Re: Dr Drool method Viable?
« Reply #66 on: February 27, 2013, 04:04:11 AM »
Quote from: %1 on February 27, 2013, 03:34:35 AM
Iso should be boiling around 253C at atmospheric pressure.
Ref:http://www.erowid.org/archive/rhodium/chemistry/isomerizafrole.html

Thanks 1% but i've seen this as stated in my post above. I believe the other isomer boils at a lower bp, and two members in this thread, myhero and pb stated that they observed boiling points around the low 240C for their iso. Just a tad of confusion, help woild be appreciated.

ImA!

Whale

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Re: Dr Drool method Viable?
« Reply #67 on: February 27, 2013, 04:42:39 AM »
Ah, my apologies. just found two different references saying that isosafrole's boiling point varies from 243-250C

hxxp://books.google.com/books?id=vxtxWneRBN4C&pg=PA1505&lpg=PA1505&dq=isosafrole+boiling+point+243+c&source=bl&ots=qNbdURMyY8&sig=MgmnrNZG9IhODFOZ5Afb4LE306o&hl=en&sa=X&ei=hI0tUfrhIcW00AGn64GQDA&ved=0CEAQ6AEwAQ#v=onepage&q=isosafrole%20boiling%20point%20243%20c&f=false

hxxp://www.zoklet.net/bbs/archive/index.php/t-56986.html
(first step to getting isosafrole tells BP)

It may be easier just to test with sulfuric. good luck

ImAMANGUYS

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Re: Dr Drool method Viable?
« Reply #68 on: February 27, 2013, 04:48:09 AM »
Quote from: %1 on February 27, 2013, 04:42:39 AM
Ah, my apologies. just found two different references saying that isosafrole's boiling point varies from 243-250C

hxxp://books.google.com/books?id=vxtxWneRBN4C&pg=PA1505&lpg=PA1505&dq=isosafrole+boiling+point+243+c&source=bl&ots=qNbdURMyY8&sig=MgmnrNZG9IhODFOZ5Afb4LE306o&hl=en&sa=X&ei=hI0tUfrhIcW00AGn64GQDA&ved=0CEAQ6AEwAQ#v=onepage&q=isosafrole%20boiling%20point%20243%20c&f=false

hxxp://www.zoklet.net/bbs/archive/index.php/t-56986.html
(first step to getting isosafrole tells BP)

It may be easier just to test with sulfuric. good luck

Cheers  ;D Never got to say welcome to the Vesp!

Enjoy

Edit: H2SO4 test revealed a brilliant red  :D Thanks.
« Last Edit: February 27, 2013, 05:11:11 AM by ImAMANGUYS »

myhero

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Re: Dr Drool method Viable?
« Reply #69 on: February 27, 2013, 10:20:18 AM »
recently as I said before i made some isosafrole and when I tried boiling it in a test tube it started boiling at around 245°C which i believe is due to the azeotrope between the the two isomers. Safrole boils at around 232°C so i rule out the possibility of having any remaining safrole in there. Any objections to my theory?

Whale

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Re: Dr Drool method Viable?
« Reply #70 on: February 27, 2013, 11:46:39 AM »
None here myhero. Seems like thats whats goin' on

pbinteger

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Some Eye Candy from the buffered performic --> Methyl Man's amalgam
« Reply #71 on: March 01, 2013, 08:55:10 PM »
1.) right after gassing in Toluene.
2.) about to filter it and wash with anhydrous acetone.
3.) another shot right before filtration.
4.) recrystallized 11 grams in boiling anhydrous IPA.
5.) up close shot of the smallish new crystals -- little needles.
6.) this is a shot of the raw / washed / dried product before recrystallization.
 :o
 ;D
« Last Edit: March 01, 2013, 08:59:15 PM by pbinteger »

Sneak

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Re: Dr Drool method Viable?
« Reply #72 on: March 02, 2013, 12:47:00 AM »
Awww man . You fucking bastard that is beautiful.. It's Friday night. I'm sat with a can of beer having a nice quiet browse and boom. Just nearly shit my pants.

Well done. Very jealous indeed. :)

What's the yield dude?
« Last Edit: March 02, 2013, 12:50:03 AM by Sneak »
If you really want to enjoy a pure, clean product the only way... is to make it yourself...

You miss 100% of the shots you don't take...

Assyl Fartrate

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Re: Dr Drool method Viable?
« Reply #73 on: March 02, 2013, 01:36:26 AM »
Great work, pbinteger.

If even bigger crystals are desired, here's the technique (for you purity freaks out there):

Get your crude heating in a small amount of the chosen solvent (in your case, IPA) - much less than necessary to dissolve your material when boiling. Once it starts boiling, slowly add more via syringe, sep funnel, or whatever you have on hand, while swirling constantly - the instant it goes fully transparent, stop, cover it, and wrap it in the thickest, most insulating material you have, and leave it on the bench for the rest of the day, then transfer it to the fridge, then the freezer (keeping it insulated the entire time). Leave it there (use the coldest setting) for a few days and you will have massive crystals - if you can resist the temptation to move it, slam the freezer door, take a peek, or disturb it in any way. Take a Buchner funnel (stored in the freezer prior, you don't want the solvent warming during the filtration!), pour everything in, and then hit the vacuum. This minimizes evaporation of solvent during the filtration process, which would inevitably deposit impurities on your otherwise beautiful and very pure crystals. If you have a nitrogen source, or can run a dehumidifier for a while, do so, as cold crystals will condense moisture in a humid atmosphere if you run the vacuum too long, and MDMA*HCl is water soluble. You don't want that.

Never tried it, but using a vacuum insulated thermos from Wal-Mart (a Dewar) may not be a bad idea.
« Last Edit: March 02, 2013, 01:49:26 AM by Assyl Fartrate »
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pbinteger

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Re: Dr Drool method Viable?
« Reply #74 on: March 03, 2013, 12:36:25 AM »
Hello,

Yields went like this:

from 700g of sassafras albidum oil 670g of isosafrole
from a 500g portion of that (glassware limitations) --> 340g of MDP-2-P
from 340g of MDP-2-P, split into 3 amalgam reactions (glassware limitations) 280g of RAW HCL MDMA.

Getting geared up now to make the last 170g of isosafrole into MDP-2-P....

_Pbint_

pbinteger

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Re: Dr Drool method Viable?
« Reply #75 on: March 03, 2013, 12:49:04 AM »
Assyl Fartrate:

I am going to try your method and post pics / results!

Thank You!

_Pbint_

ImAMANGUYS

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Re: Dr Drool method Viable?
« Reply #76 on: March 03, 2013, 12:49:41 AM »
 ;D Wow man, that looks AMAZ-BALLZ

Sneak

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Re: Dr Drool method Viable?
« Reply #77 on: March 03, 2013, 01:37:04 PM »
Wow nice work. 280g and more to go. Drool worthy. That's a a few years worth of rolling at the weekend! Have phun!

 I reckon you should have a good play around re crystallising some of that. Get some fresh crystal porn shots up. Doing it as slow as recommended sounds like you wil end up with some amazing shit.  8)

If you really want to enjoy a pure, clean product the only way... is to make it yourself...

You miss 100% of the shots you don't take...

newbiechem

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Re: Dr Drool method Viable?
« Reply #78 on: March 08, 2013, 05:18:38 AM »
Quote from: jon on December 30, 2012, 10:56:41 PM
yeah but that's just isosafrole at 89% by the time you get through all the other steps it's more like 70% overall and it's a big pain in the ass.
so i like 3 simple steps and no distillations and 90+ % yeild you can't beat that.

wow what method is that?!?!?! hehehe 3 steps, and NO DESTILATION?? im the only one never heard that?  :(

ImAMANGUYS

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Re: Dr Drool method Viable?
« Reply #79 on: March 08, 2013, 05:53:17 AM »
Quote from: newbiechem on March 08, 2013, 05:18:38 AM
Quote from: jon on December 30, 2012, 10:56:41 PM
yeah but that's just isosafrole at 89% by the time you get through all the other steps it's more like 70% overall and it's a big pain in the ass.
so i like 3 simple steps and no distillations and 90+ % yeild you can't beat that.

wow what method is that?!?!?! hehehe 3 steps, and NO DESTILATION?? im the only one never heard that?  :(

Let me direct you away from it. Though it works (backed by literature), it is difficult to get consistently high yields with it: trust me on that one. Too little too many times, But others might disagree.

If you won't believe me the method is called either the "bromosafrole" route, or commonly known in this forum as "Jon's Route."

Check it out though, learn about all the chemistry you can :D
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