Author Topic: Short Questions Thread  (Read 10825 times)

Enkidu

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 677
Re: Short Questions Thread
« Reply #580 on: July 19, 2010, 04:15:09 AM »
Anyone got any info on any of the molecules presented in the attached file?

uh, i don't think there's any hope for ANY of those

Evilblaze

  • Guest
Re: Short Questions Thread
« Reply #581 on: July 19, 2010, 10:45:13 AM »
Quote
I see that in an Erlenmeyer-Plochl will produce phenylserine

I've post a patent what describes the production of phenylerine from benzaldehyde and glycine with sodium-hydroxide catalyst.

The direct heating of benzaldehyde and gycine in toluene will produce 2 amino 1 phenylethanol, but the yield will be low. I've made this reaction long ago with alanine, but we only had a 15% yield and a large amount of black goo :-\

Also. The aminorex derivatives what you've posted maybe really bad ideas. The aminorex is a fairly good drug. Not so bad, not so good, it's just easy and relative cheap. The methylamiorex could be a nightmare if something goes wrong (we had a friend who just vomited after this compound. and why? because he smoked some weed after it).

And never forget that this drug could be easily overdosed. Mainly if there is something is mixed with it, even if this is a "simple" thing. Especially weed or psychotropic substances can cause serious problems.

Evilblaze

  • Guest
Re: Short Questions Thread
« Reply #582 on: July 25, 2010, 06:49:27 PM »
On an other forum no one replied, so:

DOI (2,5 dimethoxy 4 iodoamphetamine) is a widely used compound, lot of kids love it and they make blotters/pills from it.

The question would be, that what is the most stable DOI salt and how should this salts be stored?
And how long can be the DOI salts stored?

On an other forum someone said:
Quote
In powder form they are very stable at room temperature.
Quote
SWIM had some DOI sitting around in poor storage conditions for 15 years. It was just fine. An educated guess would be that DOC would survive lengthy storage - especially careful storage, quite well also.

The HCl salt?
Or the sulfate salt?
Or an other inorganic acid? Or an organic acid's salt?

Wich one would be the best for long time storage at room temperature?

Or maybe on blotters at room temperature?

Thanks!

java

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 783
Re: Short Questions Thread
« Reply #583 on: July 25, 2010, 07:35:25 PM »
....interesting , is there a synthesis of the compound once one has the 2,5, dimethoxybenzaldehyde?...in the other forum you mentioned.....java
¡Prefiero morir de pie que vivir siempre arrodillado!.Emiliano ZapataIt is better to die on your feet than to live on your knees!.......

Evilblaze

  • Guest
Re: Short Questions Thread
« Reply #584 on: July 25, 2010, 08:19:19 PM »
On that site there are several synthesis (wich does not work), my choice would be this:

4-Iodo-2,5-dimethoxybenzaldehyde (4)
A mixture of 2,5-dimetoxybenzaldehyde (5.10g, 30.7 mmol), silver nitrate (5.60g, 33 mmol), and iodine (8.10 g, 32 mmol) in 125
mL of methanol was stirred under nitrogen for seven hours. The yellow precipitate was filtered and
washed with methanol. The filtrate was treated dropwise with just enough saturated sodium bisulfite
solution to reduce the remaining iodine, and the solvent was removed on a rotary evaporator. The solid
was suspended with 50 mL of water, filtered, and recrystallized from 95% ethanol to yield 7.62g
(84.9%) of 4, mp 137-139°C, lit.3 mp 136-137°C.

And from this a normal amphetamine synthesis would be done, just insted benzaldehyde the 4-iodo-2,5-dimethoxy-benzaldehyde would be used. My only problem: the catalyst for the condensation of the aldehyde and the nitroethane buthylamine is used. This would react with the iodine on the phenyl ring, so I have to look for another catalyst.
Under the hydrogenation of the nitrostyrene what is the product of the condensation the iodine atom on the phenyl ring could be hydrogenated off. ArI + H2 = ArH + HI. So, this is also a little problem.
 

There is another recipe where the iodination is made on the 2,5 dimethoxy amphetamine. Here the yields are not so good, but in this case there will be no such problems, like "the iodine just disappeared from the aromatic ring".

To a solution of (R)-2,5-dimethoxyamphetamine (R)
(5.42 g, 0.028 mol) in EtOH (100 mL) was added
I2 (14.10 g, 0.066 mol) and Ag2SO4 (17.32 g, 0.066
mol) and the reaction mixture was allowed to stir
overnight. The precipitated yellow solid was collected
by filtration and the EtOH evaporated. The solid
residue was dissolved in CHCl3 and washed with
aqueous 5% NaOH (250 mL). The aqueous layer was
extracted with CHCl3 (2×300 mL) and the organic
layers were combined and washed with H2O. The
organic layer was then dried over Na2SO4, filtered,
and evaporated down to a purplish brown solid (8.45
g). Column chromatography (SiO2, 8% EtOH/CHCl3)
gave (4.31 g, 48% yield) as an off white solid.

Treatment of a CHCl3 solution of the previous compound
(6.29 g, 0.020 mol) with HCl/MeOH, followed by evaporation
of the solvent gave a solid that was recrystallized
using MeOH/Et2O. The white crystals were collected
and washed with Et2O giving R-5d hydrochloride
(5.50 g, 0.015 mol, 79% yield)

As everybody can se, the firsle obtained colored compound is just 50% pure. So this is a bit messy synthesis, but actually there is no better idea. But the yield is better than that one what is described in the PiHKAL ;D


Just an idea, but I think, that a 4-halo-2,5-dimethoxy-amphetamine thead would be useful for the forum, what do you think?

java

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 783
Re: Short Questions Thread
« Reply #585 on: July 25, 2010, 10:46:21 PM »
I think, that a 4-halo-2,5-dimethoxy-amphetamine thead would be useful for the forum, what do you think?

....i agree, so maybe you ought to start the thread and see how many will contribute ...java
¡Prefiero morir de pie que vivir siempre arrodillado!.Emiliano ZapataIt is better to die on your feet than to live on your knees!.......

no1uno

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 681
Re: Short Questions Thread
« Reply #586 on: July 31, 2010, 03:52:02 AM »
You know what, I'd agree...:| I haven't seen anything on such compounds for a coons age...

What about the B-aminoketone that can be had by the Fries rearrangement, alpha-chlorination/bromination of the acetophenone (ala Psychokitty, et al using CuBr2 or just Br2/DCM) and a Gabriel Amine synthesis?

That would "only" leave methylation, etc. wouldn't it?

There are plenty of papers (if you look around) where the B-aminoketone has been reduced with 5-10%Pd/C + 55psig/H2 to the phenethylamine, although I suppose HI could be used on it as well (prior to methylation - because it would remove the MeO groups), it has been used with other dihydroxyphenethylamines without adding to the ring (N-methyldopa springs to mind).

I personally like the look of the quaternary amines (N,N,N-trimethylphenylammonium/N,N,N,N-tetramethylammonium) for methylation, as they will only attach to the phenolic hydroxyl's (they won't touch the amine, that is why they are used to methylate morphine to codeine). Of course, you'd need to make them (or buy them), but if you have ready access to methanol (or formaldehyde) that shouldn't pose major issues.
« Last Edit: July 31, 2010, 05:41:39 AM by no1uno »
"...     "A little learning is a dang'rous thing;
    Drink deep, or taste not the Pierian spring:
    There shallow draughts intoxicate the brain,
    And drinking largely sobers us again.
..."

Vesp

  • Administrator
  • Foundress Queen
  • *****
  • Posts: 3,130
Re: Short Questions Thread
« Reply #587 on: July 31, 2010, 03:56:07 AM »
Wasn't one created? I swear I saw it around here not to long ago... :P

Edit: Ok you got me to go look for it -- http://127.0.0.1/talk/index.php/topic,1191.0.html yeah?  ;D

It went unnoticed for a bit eh?
Bitcoin address: 1FVrHdXJBr6Z9uhtiQKy4g7c7yHtGKjyLy

Quantum Dude

  • Subordinate Wasp
  • ***
  • Posts: 192
Re: Short Questions Thread
« Reply #588 on: August 02, 2010, 04:09:11 AM »


The direct heating of benzaldehyde and gycine in toluene will produce 2 amino 1 phenylethanol, but the yield will be low. I've made this reaction long ago with alanine, but we only had a 15% yield and a large amount of black goo :-\

The latter reaction was optimized by mostly Xtaldoc and I at drugs-forum a while ago. The alpha-methylserine can be obtained in very good yields without the use of a cosolvent but the decarboxylation step has yet to be handled properly.

http://www.drugs-forum.com/forum/showthread.php?t=100290
« Last Edit: August 02, 2010, 04:13:33 AM by Quantum Dude »

java

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 783
Re: Short Questions Thread
« Reply #589 on: August 02, 2010, 04:59:38 PM »
does anyone know if the synthesis of amphetamine from alpha-mehyl -trans -cinnamaldehyde  produce the d-enantiomer or the l.....since after methylation i wouldn't want to have all l -(+/-)material thanks,...java


I sort of read this but not sure yet......

http://en.wikipedia.org/wiki/Diastereomer

http://www2.chemistry.msu.edu/faculty/reusch/VirtTxtJml/sterism3.htm
« Last Edit: August 02, 2010, 05:08:32 PM by java »
¡Prefiero morir de pie que vivir siempre arrodillado!.Emiliano ZapataIt is better to die on your feet than to live on your knees!.......

Quantum Dude

  • Subordinate Wasp
  • ***
  • Posts: 192
Re: Short Questions Thread
« Reply #590 on: August 02, 2010, 05:10:47 PM »
does anyone know if the synthesis of amphetamine from alpha-mehyl -trans -cinnamaldehyde  produce the d-enantiomer or the l.....since after methylation i wouldn't want to have all l -(+/-)material thanks,...java


I sort of read this but not sure yet......

http://en.wikipedia.org/wiki/Diastereomer


The substrate does not have any optical activity to start so for sure you will obtain a racemic mixture if ''standard approaches '' are used.
« Last Edit: August 02, 2010, 05:40:11 PM by Quantum Dude »

java

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 783
Re: Short Questions Thread
« Reply #591 on: August 02, 2010, 05:19:38 PM »
if sensitive info let me now in a PM...java
« Last Edit: August 11, 2010, 03:04:35 AM by Enkidu »
¡Prefiero morir de pie que vivir siempre arrodillado!.Emiliano ZapataIt is better to die on your feet than to live on your knees!.......

Bluebottle

  • Subordinate Wasp
  • ***
  • Posts: 125
Re: Short Questions Thread
« Reply #592 on: August 10, 2010, 08:16:44 PM »
Does anyone know if there be any other, more easily acquired catalysts for the hydrogenation of tryptophan as described by Witkop (I'm pretty sure that's the one) than Pd/C? Perhaps nickel based?
"And now we divide both sides by zero..."

drone1240

  • Subordinate Wasp
  • ***
  • Posts: 105
Re: Short Questions Thread
« Reply #593 on: August 12, 2010, 03:35:54 AM »
Anybody tell me what this piece of glass is?
acting in accordance with the dictates of reason....

jon

  • Foundress Queen
  • *****
  • Posts: 1,883
Re: Short Questions Thread
« Reply #594 on: August 12, 2010, 05:38:42 AM »
i believe that is a seperator of some type used in a continuous flow process.
the what appears to be a vacum nipple is actually a hose barb and the hose is clamped and unclamped that's the function i can ascribe to it's form.
i don't believe that's pyrex either.
it says dow corning on the bottom?

embezzler

  • Subordinate Wasp
  • ***
  • Posts: 228
Re: Short Questions Thread
« Reply #595 on: August 12, 2010, 05:41:41 PM »
Aspirator Bottles with Bottom Sidearm- "These bottles are used for storing or dispensing distilled water and other laboratory solutions."

Quote from manufacturer website

All that we see or seem is but a dream within a dream...

drone1240

  • Subordinate Wasp
  • ***
  • Posts: 105
Re: Short Questions Thread
« Reply #596 on: August 13, 2010, 03:32:20 AM »
Thanks fellas. Maybe i will use it as a vase.
acting in accordance with the dictates of reason....

Oerlikon

  • Dominant Queen
  • ****
  • Posts: 365
Re: Short Questions Thread
« Reply #597 on: August 14, 2010, 03:36:45 PM »
I call it a piss-glass! ;D


Have one question on MDMA extraction...

After Al/Hg reductive amination in denat. EtOH
(temp never gone more than 55°C and reaction was left to stirr 4h after addition)
Solution was basified with equal volume of 30% NaOH, just added it with some stirring.

Now something bizarre happened, two layers separated.
Upper layer was alcoholic piss yellow cloudy with bad smell and lower one was
water ad crap.(They were separated like oil and water.)

Methylman suggested in his method to evaporate half of this alchoholic layer,
dump it in the water,extract with toluene, wash and gas it.
That failed since brown paste I got after evaporation is lousy soluble in water.

Tried A/B extraction but also failed miserably...(probably due bad solvents)

Did Al/Hg two times,same shit happened and I wasted  precious ketone.

So my question is how to eliminate this layer separation after basificatin?!
Temperature, other solvent(it is hard to find MeOH here),less/more NaOH,watch on temp....!?!?

Other thing I noticed is that MeOH/EtOH and xylene/toluene dissolve freeely in eachother,
so how is it possible to extract!? Is this possible due the high pH or what?!

Thanks!

Welcome to my lab,
where you can choose your own dreams!

Sedit

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 2,099
Re: Short Questions Thread
« Reply #598 on: August 15, 2010, 02:32:23 AM »
Will Li/Hg react simular to Na/Hg in the reduction of nitro-styrenes to amines?

Also has anyone come across a means of placing a double bond across the nitro-styrene thru reductive methylation. I fear the delocalized electron on the nitro-styrene could pose a problem for normal methylation methods.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

no1uno

  • Global Moderator
  • Foundress Queen
  • *****
  • Posts: 681
Re: Short Questions Thread
« Reply #599 on: August 22, 2010, 08:13:23 AM »
Looking for agricultural products that come as dimethylamine salts (as I am too fucking tired and sore to try and think up a decent route to dimethylamine predominantly), when I found this - MCPA (aka (4-Chloro-2-methylphenoxy)acetic acid). Comes in BIG drums (ie. 220L, 44US Gal) with ~750g/L of the dimethylamine salt.

Now, that looks like a PRIME precursor if we can get rid of the 4-chlorine - that opens up either using it as a DOM precursor (the methyl group is in place) or oxidising the methyl group to the aldehyde... If one wanted the 2CD then here is, with removal of that chlorine & the acetoxy group, the 2,5-dihydroxytoluene, methylation of which brings you to where Shulgin starts.

Alternatively, I suspect the Fries Rearrangement of the MCPA itself may actually bring you to the 4-methylacetophenone (it "should" end up ortho to ether the phenolic OH or the Cl should it not?, it certainly couldn't go para). Making use of the acid I have left over from hydrolysis of its dimethylamine salt kind of appeals.
"...     "A little learning is a dang'rous thing;
    Drink deep, or taste not the Pierian spring:
    There shallow draughts intoxicate the brain,
    And drinking largely sobers us again.
..."