Author Topic: Short Questions Thread  (Read 10826 times)

akcom

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Re: Short Questions Thread
« Reply #920 on: June 22, 2011, 02:13:11 PM »
Na/Hg is going to be the more powerful reducing agent, but for most of the chemistry we do here I'd think the Al/Hg would suffice.

Goldmember

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Re: Short Questions Thread
« Reply #921 on: June 24, 2011, 12:20:33 PM »
Sedit, or anyone for that matter,
 Yes or no: Dione to Diol with Lithium bronze?

Methyl Man

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Re: Short Questions Thread
« Reply #922 on: June 25, 2011, 09:05:12 PM »
Akcom, Pd, thank you.

Does anyone know if heptane would be an adequate alternative to toluene where toluene is used to extract from the Al/Hg/nitro reaction mixture? This toluene ban is a problem in this state, it's time to find a workable replacement. (This question assumes that the OTC heptane some of us know about hasn't been pulled as well. I need to check this out.) Thanks
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overunity33

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Re: Short Questions Thread
« Reply #923 on: June 26, 2011, 04:58:09 AM »
I don't know much more then xylene and toluene are pretty interchangeable in the reactions iv seen.

Sedit

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Re: Short Questions Thread
« Reply #924 on: June 26, 2011, 01:41:39 PM »
Looking for the density of N-Methyl-Amphetamine freebase. That MERCK page does not contain it.

Thanks for any help.
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Shake

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Re: Short Questions Thread
« Reply #925 on: June 26, 2011, 02:01:19 PM »
Quote
Akcom, Pd, thank you.

Does anyone know if heptane would be an adequate alternative to toluene where toluene is used to extract from the Al/Hg/nitro reaction mixture? This toluene ban is a problem in this state, it's time to find a workable replacement. (This question assumes that the OTC heptane some of us know about hasn't been pulled as well. I need to check this out.) Thanks

methylman,

heptane, light naptha, and the like will not suffice here.. they take tooo long to seperate from the back sludge, believe me, it took me hours and hours to sort out the big mess of solvent/sludge, when i tried naptha, which is very similar.. the weight of the aqueous is so close to the weight of the organic, that if there is any decent amount of MDMA freebase to be extracted it weighs the NP down and the two wont seperate!

check the MSDS of all your local generic thinners, i found one that was 60% tolly 40% naptha light... meanwhile xylene is priced through the roof and it always totally empty on the shelves

good thinking though, and i am loving how you are thinking outside the box, keep it up buddy

Methyl Man

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Re: Short Questions Thread
« Reply #926 on: June 27, 2011, 05:33:57 PM »
Thanks Shake, I was afraid that was the case. I'll take the credit this time for thinking outside the box, but really (in this case at least) I'm forced to by the sudden unavailability of tol and xyl. I also presume that DCM is a bad choice as well since it makes a bottom layer and one is extracting from sludgy stuff.

Strange that you refer to "black" sludge though... in the past, all the sludge I saw was battleship gray. Was yours really black? If so, that suggests an incomplete amalgamation...?

I see xylene being sold on "the bay" but it is indeed very expensive and not my preferred place to buy anything... plus I don't know whether an order would only get aborted by the seller suddenly finding that he can't ship it to CA.
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psychexplorer

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Re: Short Questions Thread
« Reply #927 on: June 27, 2011, 06:09:34 PM »
Thanks Shake, I was afraid that was the case. I'll take the credit this time for thinking outside the box, but really (in this case at least) I'm forced to by the sudden unavailability of tol and xyl. I also presume that DCM is a bad choice as well since it makes a bottom layer and one is extracting from sludgy stuff.

Strange that you refer to "black" sludge though... in the past, all the sludge I saw was battleship gray. Was yours really black? If so, that suggests an incomplete amalgamation...?

I see xylene being sold on "the bay" but it is indeed very expensive and not my preferred place to buy anything... plus I don't know whether an order would only get aborted by the seller suddenly finding that he can't ship it to CA.

I don't want to take this too far off track, but have you looked at various OTC formulations of mixed solvents which might contain assorted methylbenzenes?

Barring that, toluene and xylene are available online from an enormous variety of smaller stores across an enormous variety of product uses. Many of these sellers are small businesses outside your state. Since possession of toluene is still legal, and not controlled like drugs or weapons, you won't find interstate barriers to shipping, nor would most small businesses even maintain a compliance department to figure out what solvents are legal under what conditions in what states. A ban on retail sales of toluene solvents in California won't affect the behavior of a model hobby outlet shipping from Iowa. That business sees plenty of online solvent orders and might even sympathize with customers whose hobbies are being curtailed by heavy handed bureaucrats.

Shopping search portals are great ways to find common solvents. Another good technique is a Google query such as "toluene gallon" (+ some sort of sale language), which will sort out mentions of your chosen solvent among pages which aren't offering a specified quantity for sale.

The bay should definitely be out, though.

RoidRage

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Re: Short Questions Thread
« Reply #928 on: June 27, 2011, 06:37:40 PM »
Looking for the density of N-Methyl-Amphetamine freebase. That MERCK page does not contain it.

Thanks for any help.

Chemspider states it's 0.907g/ml


Sedit

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Re: Short Questions Thread
« Reply #929 on: June 27, 2011, 08:13:11 PM »
Thanks roid, I didn't even think to check chemspider.
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Shake

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Re: Short Questions Thread
« Reply #930 on: June 28, 2011, 05:33:22 AM »
Quote
I also presume that DCM is a bad choice as well since it makes a bottom layer and one is extracting from sludgy stuff.

DCM extracting here is the biggest bitch, as you are right, it sits on the bottom, but it also forms an azeotrope with the methanol, and you get this one big homogenous sludge, so you are right DCM here is not good either.. i learned both of these the hard way..

most otc thinners contain toluene, as i said go through thier MSDS youll find one that is a nice mix of naptha and toluene, i found it did the trick

Quote
Strange that you refer to "black" sludge though... in the past, all the sludge I saw was battleship gray. Was yours really black? If so, that suggests an incomplete amalgamation...?


I found it varys with the amount of aluminum.. i always took a darker and stinkier sludge as a good sign of a successful reaction. when i hit it with NaOH and i dont get dark, im about ready to give up then and there! worst feeling

Also, i have always taken a nice steel blue tint as a sign of success before basifying with the couple litres of base, this only would come from stirring the amalgum sludge for a good 10 - 12 hours before adding the NaOH, 6 never seems to be enough judging by the look of it

but i played around with the ratios, im willing to bet yours are pretty close to the mark as written.. in fact i know they are
« Last Edit: June 28, 2011, 05:38:50 AM by Shake »

hoax

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Re: Short Questions Thread
« Reply #931 on: July 03, 2011, 03:34:31 PM »
Recently I've found interesting paper describing hydrobromination of various alkenes on silica: http://www.scielo.br/pdf/jbchs/v12n5/a13v12n5.pdf
Quote
The reaction of several alkenes with 0.4 mol equiv. PBr3/SiO2 in dichloromethane at room temperature gave the alkyl bromides with Markovnikov regiospecificity in 50 - 100% yield and short reaction time.


I'd like to try it on some stuff from essential oils, but up here even HCl is a controlled precursor. I was wondering whether I could hydrolyse FeCl3 in DCM, dehydrate it with CaCl2 and use it instead of HCl or its precursors mentioned in the paper. I couldn't find any info on iron/ferrous hydroxide solubility in DCM, will it precipitate? Any other ideas? I'd love to keep it as OTC as possible and avoid messing with gaseous HCl.

Terror

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Re: Short Questions Thread
« Reply #932 on: July 05, 2011, 09:30:48 AM »
Been offered some equipment..

Anyone know anything about edwards speedivac vacuum pumps? pulls to 0.05 tor =)

And.. the bigger questions, can an ion chromatography system be adapted to a o-chem  with a UV detector?

Im specifically looking at a Dionex DX500 with gradient pump, column temperature stabiliser and auto-sampler  a variety of accessories and consumables, a set of manuals and Peaknet software for a price so low my momma couldn't even buy tampons.
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sassa

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Re: Short Questions Thread
« Reply #933 on: July 05, 2011, 02:21:55 PM »
ONLY TWO QUEsTIONS:
   -Any idea about MDMA and MDA  freebase distillation temperatures,both about atmospheric temperature and with a vacuum that boils safrole aprox.(95-110),ketone (130-150º)....some advice about cares with that distillation?....ant too,....how to store it for future gas treating....can one store the freebase for moths well sealed...on frezer...or must be into a solvent??...Not too much info on the web about freebase properties.
   - About gassing on dry  freezed acetone(ala old school)?....read can be tricky(about h20 i supossed) and posible dangerous,but don´t remember about what gas formed,it´s posible?.Reason:i can buy pure acetone locally very cheap....but have to order both DCM and Toluene and seems hard to re-use after gassing.
   Cheers!

overunity33

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Re: Short Questions Thread
« Reply #934 on: July 05, 2011, 05:51:27 PM »
but up here even HCl is a controlled precursor.

wtf? which area are you from?

Methyl Man

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Chromatography
« Reply #935 on: July 15, 2011, 02:31:42 AM »
Hi guys,

My associate asked me a question about chromatography which I pass onto you in hopes you can offer info. (I think he's referring to thin-film chromatography but I don't know. He mentioned having a chromatography tank, if that helps)

Did you see any mention of glass plate chromatography assessments in any of the forums you read?  If so, see what solvent is recommended and the type of chromatography plate they use.

big thanks,
MM
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Wizard X

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Re: Chromatography
« Reply #936 on: July 15, 2011, 03:05:29 AM »
Hi guys,

My associate asked me a question about chromatography which I pass onto you in hopes you can offer info. (I think he's referring to thin-film chromatography but I don't know. He mentioned having a chromatography tank, if that helps)

Did you see any mention of glass plate chromatography assessments in any of the forums you read?  If so, see what solvent is recommended and the type of chromatography plate they use.

big thanks,
MM
Use the glass plates out of picture frames for the 1D, or 2D, glass plate chromatography.

Read this: http://www.chromsource.com/books/Milestones-TLC.pdf

1D & 2D glass plate chromatography. Two-dimensional planar chromatography with a closed adsorbent layer.

A new two-dimensional chromatography process on closed plates is proposed. A previously described device with ethanol as a mobile phase is used to experimentally study two-dimensional thin-layer chromatography (2D TLC) on plates with 5 × 5 and 10 × 10 cm sizes. This work includes the experimental study and comparison of the following TLC versions: (1) the proposed 2D TLC version with a closed adsorbent layer with 1D separation on closed plates (an ascending mobile phase flow) and (2) conventional 2D TLC with an open adsorbent layer. The ascending version of 2D TLC with a closed adsorbent layer considerably (by ?55%) shortens the chromatographic time, especially with the use of 5 × 5 cm plates in the 2D separation version compared with the 1D version on 10 × 10 cm plates.

http://www.springerlink.com/content/f6627415u0773138/

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Enkidu

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Re: Chromatography
« Reply #937 on: July 15, 2011, 03:16:22 AM »
If so, see what solvent is recommended and the type of chromatography plate they use.[/i]

The solvent is called the eluent, and the choice of eluent depends on the analyte (or whatever they call it in preparative chromatography).

Bardo

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Elemicin from Gallic Acid
« Reply #938 on: July 15, 2011, 04:15:09 PM »
Anybody have the synthesis for elemicin from gallic acid? I have found the synthesis's for mescaline from gallic acid but I can't find the synthesis for elemicin from gallic acid anywhere..... On a side note anyone have any ideas on solidifying a phenylpropene? Thanks.


^^^ Above reposted after getting removed by Enkidu's censoring happy fingers. If you want a reference Enkidu how about "Studies on Elemicin Synthesis" by Dorothy Huang Hains published by McNeese State University in 1976. It has the synthesis for elemicin from gallic acid in it, the only problem is from what I can tell there are only two copies of this 60 page book and they are both in McNeese State University's library.

Enkidu

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Re: Short Questions Thread
« Reply #939 on: July 15, 2011, 06:17:55 PM »
I'll see whether I can get the thesis. As such, it's a book as much as your diary is a book, in that it is bound. Next time, request references in the appropriate thread and by using the appropriate citation.