Author Topic: Short Question Thread 2.0  (Read 5704 times)

Electro┬┤S

  • Pupae
  • **
  • Posts: 95
Re: Short Question Thread 2.0
« Reply #340 on: March 30, 2013, 02:14:50 AM »
Finally i think. He wants say a balanced addition funnel instead of soxhlet capsule.
It would be a RBF with the ethanol nitrostyrene mix at reflux with the NaBH4 in the funnel and the condenser at the top of the funnel.
Then the NaBH4 is added to the reaction dissolved in the condensed ethanol drops.
 8)


Electro┬┤S

  • Pupae
  • **
  • Posts: 95
Re: Short Question Thread 2.0
« Reply #341 on: March 30, 2013, 02:23:57 AM »
Ok, ok. This guy is talking about break the syphon part from a Soxhlet capsule. He he, i had need a little of time . ::)

Tsathoggua

  • Autistic sociopath
  • Foundress Queen
  • *****
  • Posts: 662
Re: Short Question Thread 2.0
« Reply #342 on: March 30, 2013, 02:59:10 AM »
Can HBr (room temp, 15% in GAA) be used successfully for ether cleavage of oxycodone to oxymorphone? if so, what are the yields like?

And my other quick question is this-Toady has been told on here that oxycodone esters are not worth bothering with. Does the same hold true for 6-position esters, or 3,6-diesters of oxymorphone? (talking about the enol ester here at the 3-position carbonyl)
« Last Edit: March 30, 2013, 04:06:36 AM by Tsathoggua »
Nomen mihi Legio est, quia multi sumus

I'm hyperbolic, hypergolic, viral, chiral. So motherfucking twisted my laevo is on the right side.

b6baddawg

  • Larvae
  • *
  • Posts: 35
Re: Short Question Thread 2.0
« Reply #343 on: April 02, 2013, 01:09:10 AM »
Am i missing something or can tma-2 be gotton too following this,
veratraldehyde (3,4-dimethoxybenzaldehyde) > to (2-Bromo-4,5-dimethoxybenzaldehyde) > to 2,4,5-Trimethoxyphenyl-2-nitropropene > tma-2?

The reactions would be, from veratraldehyde http://www.erowid.org/archive/rhodium/chemistry/tma2.vanillin.html giving the 2-bromo-4,5 then what im unsure is can i go directly to the tma-p2np using pihkal 157 procedure
http://www.erowid.org/library/books_online/pihkal/pihkal157.shtml
(shulgins use of n-butylamine gives higher yield in the 157 procedure than the example in 158 using ammonium acetate)

bjuice

  • Pupae
  • **
  • Posts: 59
Re: Short Question Thread 2.0
« Reply #344 on: April 09, 2013, 08:16:14 PM »
Hello Vespiary!

Just finished my first al/hg nitro reduction and am a little concerned because my toluene extraction came out with a deep yellow colour, whereas the pictorials I've seen both have their extractions come out colorless. So I'm assuming unreacted mdp2p, or maybe some other reaction byproducts. The reaction itself, as far as I can tell, went exactly as it should.

Either way, I'm conflicted on how to best work this up. I've already done my washes and have the organic layer drying over cacl2 at the moment. Now I'm trying to decide between

a) gassing with hcl
b) acid base workup, then gas. ie: wash organic layer with hcl/water, discard organic, basify aqueous, bring into fresh toluene. Then dry and gas.

Any thoughts on this?
« Last Edit: April 09, 2013, 08:22:01 PM by bjuice »

fractal

  • Subordinate Wasp
  • ***
  • Posts: 110
Re: Short Question Thread 2.0
« Reply #345 on: April 09, 2013, 10:06:51 PM »
May just be from an impurity in your MDP-2-P. You should gas it and see if you get MDMA HCl. Very easy to clean up from there provided you get crystals.

bjuice

  • Pupae
  • **
  • Posts: 59
Re: Short Question Thread 2.0
« Reply #346 on: April 10, 2013, 12:38:54 AM »
Hello Vespiary!

Just finished my first al/hg nitro reduction and am a little concerned because my toluene extraction came out with a deep yellow colour, whereas the pictorials I've seen both have their extractions come out colorless. So I'm assuming unreacted mdp2p, or maybe some other reaction byproducts. The reaction itself, as far as I can tell, went exactly as it should.

Either way, I'm conflicted on how to best work this up. I've already done my washes and have the organic layer drying over cacl2 at the moment. Now I'm trying to decide between

a) gassing with hcl
b) acid base workup, then gas. ie: wash organic layer with hcl/water, discard organic, basify aqueous, bring into fresh toluene. Then dry and gas.

Any thoughts on this?

Gassed the toluene and....crystals!  A whopping 3 grams from 45 grams mdp2p.  I'm stoked that I've produced my first ever MDMA, but sad at the low yields.  Luckily I'm working through another batch as we speak.

I'm going to wash the toluene with water in hopes that it's not completely dry, and has MDMA locked up in it.

zgoat65

  • Subordinate Wasp
  • ***
  • Posts: 103
Re: Short Question Thread 2.0
« Reply #347 on: April 10, 2013, 12:48:55 AM »
Maybe add some bisulfite or metabisulfite to see if you have any ketone present.  Also a good way to seperate.
If you build a man a fire, he'll be warm for a day.
If you set a man on fire, he'll be warm for the rest of his life

bjuice

  • Pupae
  • **
  • Posts: 59
Re: Short Question Thread 2.0
« Reply #348 on: April 10, 2013, 12:59:28 AM »
Don't have any bisulfite on hand, but..

The water wash is looking GOOD.  The aqueous layer instantly became cloudy as I watched crystal cascade from the organic layer to the aqueous.  Scratch what I said about evaporating.  Going to wash aqueous with clean toluene, separate, then basify the water to see if any oil drops out.
« Last Edit: April 10, 2013, 01:09:31 AM by bjuice »

bjuice

  • Pupae
  • **
  • Posts: 59
Re: Short Question Thread 2.0
« Reply #349 on: April 10, 2013, 01:30:48 AM »
Added NaOH to the water and it turned to what appears to be milk.  Going to let it sit.

Aaand I'm accidentally rolling.  Remind me to wear gloves next time I scrape the filter paper  ;D

Guess I'll be reporting back later with results.  Any input on the workup situation would be greatly appreciated!

bjuice

  • Pupae
  • **
  • Posts: 59
Re: Short Question Thread 2.0
« Reply #350 on: April 10, 2013, 02:24:35 AM »
Washed the milky aqueous layer with clean toluene and a horrible looking emulsion formed, complete with what appears to be small plasticky flakes that won't dissolve in either layer.  I think I may be beating a dead horse here :(

Edit: Separated layers and discarded aqueous.  Filtered toluene through a buchner to remove the polymerized crap.  Washed with 10% HCl/H2O, which is now evaporating.  Don't wanna take my chances with gassing again.
« Last Edit: April 10, 2013, 03:44:34 AM by bjuice »

fractal

  • Subordinate Wasp
  • ***
  • Posts: 110
Re: Short Question Thread 2.0
« Reply #351 on: April 10, 2013, 03:40:57 PM »
Sounds like you had some amine in your HCl/Water layer. Should have just evaporated of the water and recrystallized.

Flight

  • Larvae
  • *
  • Posts: 23
Re: Short Question Thread 2.0
« Reply #352 on: April 10, 2013, 07:56:30 PM »
 I need some help understanding this, "Place the safrole (purified by simple distillation under vacuum) along with 2-5% KOH under good stirring.  I use about 2.5% and it works like a charm." 

How do you determine what amount in grams 2-5% KOH is?

I apologize if this is obvious, but I need some assistance. 

bjuice

  • Pupae
  • **
  • Posts: 59
Re: Short Question Thread 2.0
« Reply #353 on: April 10, 2013, 08:13:51 PM »
Sounds like you had some amine in your HCl/Water layer. Should have just evaporated of the water and recrystallized.

Agreed.  The aqueous layer finished evaporating and left me with a honey-colored oil.  Not sure if there's any of the goodies in the oil, or how I would go about finding out.

fractal

  • Subordinate Wasp
  • ***
  • Posts: 110
Re: Short Question Thread 2.0
« Reply #354 on: April 10, 2013, 08:29:11 PM »
@ flight-2-5% based on the number of moles of safrole you are trying to isomerize. So if you are trying to isomerize 1.25mol of safrole you need .0313mol of KOH, calculate it like this:

1.25mol safrole x.025 = .0313mol KOH

From there you just convert moles back into grams by multiplying the answer by the molar mass of KOH.

fractal

  • Subordinate Wasp
  • ***
  • Posts: 110
Re: Short Question Thread 2.0
« Reply #355 on: April 10, 2013, 08:33:22 PM »
Agreed.  The aqueous layer finished evaporating and left me with a honey-colored oil.  Not sure if there's any of the goodies in the oil, or how I would go about finding out.

Let it dry as much as possible and recrystallize in a small amount of anhydrous acetonitrile.

Flight

  • Larvae
  • *
  • Posts: 23
Re: Short Question Thread 2.0
« Reply #356 on: April 10, 2013, 08:58:32 PM »
@ fractal- "2-5% based on the number of moles of safrole you are trying to isomerize. So if you are trying to isomerize 1.25mol of safrole you need .0313mol of KOH, calculate it like this:

1.25mol safrole x.025 = .0313mol KOH

From there you just convert moles back into grams by multiplying the answer by the molar mass of KOH."

So g/mol of KOH is 56.1056 x .0313 = 1.75g KOH right?

1.25mol safrole is 1.25 x 162.19 = 202g of safrole

Thanks for your help Fractal

bjuice

  • Pupae
  • **
  • Posts: 59
Re: Short Question Thread 2.0
« Reply #357 on: April 10, 2013, 11:35:00 PM »
Agreed.  The aqueous layer finished evaporating and left me with a honey-colored oil.  Not sure if there's any of the goodies in the oil, or how I would go about finding out.

Let it dry as much as possible and recrystallize in a small amount of anhydrous acetonitrile.

It's been drying all day and is starting to form crystals!  Not nearly as much as I'd hoped, but still a substantial amount.  I don't have acetonitrile.  Am I right in thinking that I can recrystallize in IPA?

fractal

  • Subordinate Wasp
  • ***
  • Posts: 110
Re: Short Question Thread 2.0
« Reply #358 on: April 11, 2013, 12:05:13 AM »
Yeah, there are a bunch of different solvents that will get the job done.

bjuice

  • Pupae
  • **
  • Posts: 59
Re: Short Question Thread 2.0
« Reply #359 on: April 11, 2013, 01:04:22 AM »
Great thanks fractal.